USP《671》美国药典-包装容器——性能检测译文

231 HEAVY METALS重金属This test is provided to demonstrate that the content of metallic impurities that are colored by sulfide ion, under the specified test conditions, does not exceed the Heavy metals limit specified in the individual monograph in percentage (by weight） of lead in the test substance， as determined by concomitant visual comparison （see Visual Comparison in the section Procedure under Spectrophotometry and Light—Scattering（851) with a control prepared from a Standard Lead Solution。

［NOTE-Substances that typically will respond to this test are lead， mercury, bismuth, arsenic，antimony， tin， cadmium, silver, copper， and molybdenum. ]本检验是用来测定与硫化物离子作用显色的金属杂质含量，在规定检验条件下，其检测结果不得超过专论中规定的重金属限度供试品中铅的百分比（重量比）,该检验是通过与标准铅溶液配制的对照进行视觉比较来得出结论的(参看分光光度法和光散射法<851>中规程部分的视觉比较）.［注意：与本检验起反应的代表性物质为铅、汞、铋、砷、锑、锡、镉、银、铜和钼。

《671》包装容器——性能检测本章规定了用来包装的塑料容器及其组件功能性质上的标准(药品、生物制剂、营养补充剂和医疗器械)，定义了保存、包装、存储和标签方面的凡例与要求。

本文提供的试验用于确定塑料容器的透湿性和透光率。

盛装胶囊和片剂的多单元容器章节适用于多单元容器。

盛装胶囊和片剂的单位剂量容器章节适用于单位剂量容器。

盛装胶囊和片剂的多单元容器(没有密封) 的章节适用于没有密封的聚乙烯和聚丙烯容器。

盛装液体的多元和单元容器的章节适用于多元的和单元的容器。

一个容器想要提供避光保护或作为一个符合耐光要求的容器，由具有耐光的特殊性质的材料组成，包括任何涂层应用。

一个无色透明或半透明的容器通过一个不透明的外壳包装变成耐光的(见凡例和要求 )，可免于对光的透射要求。

在多单元容器和封盖与水泡的单位剂量容器由衬垫密封情况下，此处使用的术语“容器”指的是整个系统的组成。

盛装胶囊和片剂的多元容器干燥剂——放置一些颗粒4—8目的无水氯化钙在一个浅的容器里，仔细剔除细粉，然后置于110°干燥，并放在干燥器中冷却。

试验过程——挑选12个类型和尺寸一致的容器，用不起毛的毛巾清洁密闭表面，并打开和关闭每个容器30次。

坚决每次应用容器密闭一致。

通过扭矩关闭螺旋盖容器，使气密性在附表规定的范围内。

10个指定的测试容器添加干燥剂，如果容器容积大于等于20mL，每个填充13mm以内封闭；如果容器的容积小于20毫升，每个填充容器容量的三分之二。

如果容器内部的深度超过63mm，惰性填料或垫片可以放置在底部来最小化容器和干燥剂的总重量；干燥剂层在这样一个容器中深度不低于5cm。

添加干燥剂之后，立即按附表中规定的扭矩封闭螺旋帽容器。

剩余的2个指定为对照容器，每个添加足够数量的玻璃珠，重量约等于每个测试容器的重量，并用附表中规定的扭矩封闭螺旋帽容器。

记录各个容器的重量，如果容器的容积小于20毫升，精确到0.1毫克；如果容器容积为20毫升或以上但小于200毫升，精确到毫克；如果容器容积为200毫升及以上，精确到厘克（10毫克）；在相对湿度75±3%和温度23±2°的环境下存储。

USP38通用章节目录中文USP38-通用章节指导目录(附录)Guide to General Chapters 通用章节指导General Requirements for Test and Assays检查与含量分析的一般要求＜1＞INJECTIONS AND IMPLANTED DRUG PRODUCTS (PARENTERALS)—PRODUCT QUALITY TESTS 注射和植入药物产品(注射用) —产品质量测试＜1＞INJECTIONS注射剂＜2＞ORAL DRUG PRODUCTS—PRODUCT QUALITY TESTS 口服药物产品质量测试＜3＞TOPICAL AND TRANSDERMAL DRUG PRODUCTS—PRODUCT QUALITY TESTS 局部和透皮药物产品—产品质量测试＜4＞MUCOSAL DRUG PRODUCTS—PRODUCT QUALITY TESTS 粘膜药物产品质量测试＜5＞INHALATION AND NASAL DRUG PRODUCTS—GENERAL INFORMATION AND PRODUCT QUALITY TESTS 吸入剂产品—产品质量测试＜7＞LABELING 标签＜11＞USP REFERENCE STANDARDS USP标准品Apparatus for Test and Assays用于检查与含量分析的器具＜17＞PRESCRIPTION CONTAINER LABELING处方容器标签＜21＞THERMOMETERS温度计＜31＞VOLUMETRIC APPARATUS容量器具＜41＞BALANCES天平Microbiological Tests 微生物检查法＜51＞ANTIMICROBIAL EFFECTIVENESS TESTING抗菌剂有效性检查法＜55＞BIOLOGICAL INDICATORS—RESISTANCE PERFORMANCE TESTS生物指示剂－耐药性实验＜61＞MICROBIOLOGICAL EXAMINATION OF NONSTERILE PRODUCTS: MICROBIAL ENUMERATION TESTS非无菌产品的微生物限度检查：微生物列举检查法＜62＞MICROBIOLOGICAL EXAMINATION OF NONSTERILE PRODUCTS: TESTS FOR SPECIFIED MICROORGANISMS 非无菌产品的微生物限度检查：特定微生物检查法＜63＞MYCOPLASMA TESTS 支原体检查法＜71＞STERILITY TESTS无菌检查法Biological tests and assays生物检查法与测定法＜81＞ANTIBIOTICS—MICROBIAL ASSAYS抗生素－微生物测定＜85＞BACTERIAL ENDOTOXINS TEST细菌内毒素检查法＜87＞BIOLOGICAL REACTIVITY TESTS, IN VITRO体外的生物反应性检查法＜88＞BIOLOGICAL REACTIVITY TESTS, IN VIVO 体内的生物反应性检查法＜89＞ENZYMES USED AS ANCILLARY MATERIALS IN PHARMACEUTICAL MANUFACTURING 药品生产中酶作为辅料所使用＜90＞FETAL BOVINE SERUM—QUALITY ATTRIBUTES AND FUNCTIONALITY TESTS 牛胎儿血清-质量品质和功能检查法＜91＞CALCIUM PANTOTHENATE ASSAY泛酸钙测定法＜92＞GROWTH FACTORS AND CYTOKINES USED IN CELL THERAPY MANUFACTURING 在细胞疗法中使用生长因子和细胞因子＜111＞DESIGN AND ANALYSIS OF BIOLOGICAL ASSAYS 生物测定法的设计与分析＜115＞DEXPANTHENOL ASSAY右泛醇（拟胆碱药）测定法＜121＞INSULIN ASSAYS胰岛素测定法＜121.1＞PHYSICOCHEMICAL ANALYTICAL PROCEDURES FOR INSULINS胰岛素的物理化学分析程序＜123＞GLUCAGON BIOIDENTITY TESTS 高血糖素的生物鉴别检查法＜124＞ERYTHROPOIETIN BIOASSAYS 红细胞生成素的微生物测定＜126＞SOMATROPIN BIOIDENTITY TESTS 生长激素的生物鉴别检查法＜130＞PROTEIN A QUALITY ATTRIBUTES 蛋白质A的质量特征＜151＞PYROGEN TEST热原检查法＜161＞TRANSFUSION AND INFUSION ASSEMBLIES AND SIMILAR MEDICAL DEVICES 输血输液用具以及相类似的医疗器械＜171＞VITAMIN B12 ACTIVITY ASSAY……2548维生素B12活性测定法Chemical Tests and assays化学实验检查与测定法鉴别检查＜181＞IDENTIFICATION—ORGANIC NITROGENOUS BASES 鉴别－有机氮碱化合物＜191＞IDENTIFICATION TESTS—GENERAL鉴别实验－通用＜193＞IDENTIFICATION—TETRACYCLINES鉴别－四环素类＜197＞SPECTROPHOTOMETRIC IDENTIFICATION TESTS分光光度计鉴别实验＜201＞THIN-LAYER CHROMATOGRAPHIC IDENTIFICATION TEST薄层色谱鉴别实验Limit Tests 限度检查法＜206＞ALUMINUM铝＜207＞TEST FOR 1,6-ANHYDRO DERIV ATIVE FOR ENOXAPARIN SODIUM依诺肝素钠的酐类衍生物实验＜208＞ANTI-FACTOR Xa AND ANTI-FACTOR IIa ASSAYS FOR UNFRACTIONATED AND LOW MOLECULAR WEIGHT HEPARINS 普通肝素和低分子肝素产品中抗体Xa和抗体IIa测定＜209＞LOW MOLECULAR WEIGHT HEPARIN MOLECULAR WEIGHT DETERMINATIONS 低分子肝素钠分子量测定＜211＞ARSENIC砷＜221＞CHLORIDE AND SULFATE氯和硫＜223＞DIMETHYLANILINE二甲基苯胺＜226＞4-EPIANHYDRO-TETRACYCLINE4－？－四环素＜227＞4-AMINOPHENOL IN ACETAMINOPHEN-CONTAINING DRUG PRODUCTS 对乙酰氨酚药物产品中氨基酚＜228＞ETHYLENE OXIDE AND DIOXANE 环氧乙烷和二氧六环＜231＞HEA VY METALS重金属（删除）＜232＞ELEMENTAL IMPURITIES—LIMITS 元素杂质-限度＜233＞ELEMENTAL IMPURITIES—PROCEDURES 元素杂质-规程＜241＞IRON铁＜251＞LEAD铅＜261＞MERCURY汞＜267＞POROSIMETRY BY MERCURY INTRUSION 水银孔隙仪＜268＞POROSITY BY NITROGEN ADSORPTION–DESORPTION 氮吸附-解吸测定孔隙率＜271＞READILY CARBONIZABLE SUBSTANCES TEST易碳化物检查法＜281＞RESIDUE ON IGNITION炽灼残渣＜291＞SELENIUM硒Other Tests and Assays 其它检查法与测定法＜301＞ACID-NEUTRALIZING CAPACITY酸中和容量＜311＞ALGINATES ASSAY藻酸盐测定法＜341＞ANTIMICROBIAL AGENTS—CONTENT 抗菌剂－含量＜345＞Assay for Citric Acid/Citrate and Phosphate 柠檬酸/柠檬酸盐和磷酸盐的测定＜351＞ASSAY FOR STEROIDS类固醇（甾类化合物）测定法＜361> BARBITURATE ASSAY 巴比妥类药物测定法＜371＞COBALAMIN RADIOTRACER ASSAY钴铵素放射性跟踪剂测定法＜381＞ELASTOMERIC CLOSURES FOR INJECTIONS 注射剂的弹性密封件＜391＞EPINEPHRINE ASSAY肾上腺素测定法＜401＞FATS AND FIXED OILS脂肪与混合油＜411＞FOLIC ACID ASSAY叶酸测定法＜413＞IMPURITIES TESTING IN MEDICAL GASES 医用气体杂质检查＜415＞MEDICAL GASES ASSAY 医用气体含量检查＜425＞IODOMETRIC ASSAY—ANTIBIOTICS碘量检查法－抗生素＜429＞LIGHT DIFFRACTION MEASUREMENT OF PARTICLE SIZE粒径的光衍射测量法＜431＞METHOXY DETERMINATION甲氧基测定法＜441＞NIACIN OR NIACINAMIDE ASSAY 烟酰或烟酰胺测定法＜451＞NITRITE TITRATION亚硝酸盐滴定＜461＞NITROGEN DETERMINATION氮测定法＜466＞ORDINARY IMPURITIES一般杂质＜467＞RESIDUAL SOLVENTS残留溶剂＜469＞ETHYLENE GLYCOL, DIETHYLENE GLYCOL, AND TRIETHYLENE GLYCOL IN ETHOXYLATED SUBSTANCES乙氧基物质中乙二醇、二甘醇、三甘醇测定＜471＞OXYGEN FLASK COMBUSTION氧瓶燃烧法＜481＞RIBOFLAVIN ASSAY核黄素（维生素B2）测定法＜501＞SALTS OF ORGANIC NITROGENOUS BASES有机氮盐＜503＞ACETIC ACID IN PEPTIDES 多肽类中乙酸测定＜511＞SINGLE-STEROID ASSAY单一的类固醇测定法＜525＞SULFUR DIOXIDE 二氧化硫＜531＞THIAMINE ASSAY硫胺素测定法＜541＞TITRIMETRY滴定法＜551＞VITAMIN E ASSAY维生素E测定法＜561＞ARTICLES OF BOTANICAL ORIGIN植物起源的药品＜563＞IDENTIFICATION OF ARTICLES OF BOTANICAL ORIGIN植物药品的鉴别＜565＞BOTANICAL EXTRACTS植物提取＜571＞VITAMIN A ASSAY维生素A测定法＜581＞VITAMIN D ASSAY维生素D测定法＜591＞ZINC DETERMINATION锌的测定法Physical Test and Determinations物理检查与测定法＜601＞INHALATION AND NASAL DRUG PRODUCTS: AEROSOLS, SPRAYS, AND POWDERS—PERFORMANCE QUALITY TESTS吸入剂、鼻雾剂：气溶胶，喷雾，干粉-质量通则＜602＞PROPELLANTS 推进剂＜603＞TOPICAL AEROSOLS 局部喷雾剂＜604＞LEAK RATE 渗漏率＜610＞ALTERNATIVE MICROBIOLOGICAL SAMPLING METHODS FOR NONSTERILE INHALED AND NASAL PRODUCTS 非无菌吸入和鼻雾剂可供选择的微生物取样方法＜611＞ALCOHOL DETERMINATION乙醇测定法＜616＞BULK DENSITY AND TAPPED DENSITY堆密度与振实密度＜621＞CHROMATOGRAPHY色谱法＜631＞COLOR AND ACHROMICITY呈色与消色＜641＞COMPLETENESS OF SOLUTION溶解度＜643＞TOTAL ORGANIC CARBON总有机碳＜645＞W ATER CONDUCTIVITY水电导率＜651＞CONGEALING TEMPERATURE凝点温度＜659＞PACKAGING AND STORAGE REQUIREMENTS 包装和储藏要求＜660＞CONTAINERS—GLASS 容器-玻璃＜661＞CONTAINERS—PLASTICS容器-塑料＜670＞AUXILIARY PACKAGING COMPONENTS 辅助包装部件＜671＞CONTAINERS—PERFORMANCE TESTING容器－性能测试＜691＞COTTON棉花＜695＞CRYSTALLINITY结晶度＜696＞CHARACTERIZATION OF CRYSTALLINE SOLIDS BY MICROCALORIMETRY AND SOLUTION CALORIMETRY 通过溶液量热学测定结晶性＜697＞CONTAINER CONTENT FOR INJECTIONS 注射剂容器容积＜698＞DELIVERABLE VOLUME抽取体积＜699＞DENSITY OF SOLIDS固体密度＜701＞DISINTEGRATION崩解时限＜705＞QUALITY ATTRIBUTES OF TABLETS LABELED AS HA VING A FUNCTIONAL SCORE ？＜711＞DISSOLUTION 溶出度＜721＞DISTILLING RANGE馏程＜724＞DRUG RELEASE药物释放度＜729＞GLOBULE SIZE DISTRIBUTION IN LIPID INJECTABLEEMULSIONS脂类可注射的乳剂的粒径分布＜730＞Plasma Spectrochemistry 血浆光谱化学？＜731＞LOSS ON DRYING4干燥失重＜733＞LOSS ON IGNITION灼烧失重＜735＞X-RAY FLUORESCENCE SPECTROMETRY X射线光谱＜736＞MASS SPECTROMETRY 质谱＜741＞MELTING RANGE OR TEMPERATURE熔距或熔点＜751＞METAL PARTICLES IN OPHTHALMIC OINTMENTS眼用软膏中的金属粒子＜755＞MINIMUM FILL最低装量＜761＞NUCLEAR MAGNETIC RESONANCE核磁共振＜771＞OPHTHALMIC OINTMENTS眼用软膏＜776＞OPTICAL MICROSCOPY光学显微镜＜781＞OPTICAL ROTATION旋光度＜785＞OSMOLALITY AND OSMOLARITY渗透压＜786＞PARTICLE SIZE DISTRIBUTION ESTIMATION BY ANALYTICAL SIEVING 筛分法估算粒径分布＜787＞SUBVISIBLE PARTICULATE MATTER IN THERAPEUTIC PROTEIN INJECTIONS显微计数法在治疗性蛋白注射剂中应用＜788＞PARTICULATE MATTER IN INJECTIONS注射剂中的不溶性微粒＜789＞PARTICULATE MATTER IN OPHTHALMIC SOLUTIONS 眼用溶液中的不溶性微粒＜790＞VISIBLE PARTICULATES IN INJECTIONS 注射剂中可见异物＜791＞pH＜795＞PHARMACEUTICAL COMPOUNDING—NONSTERILE PREPARATIONS药物混合－非无菌制剂＜797＞PHARMACEUTICAL COMPOUNDING—STERILE PREPARATIONS药物混合－无菌制剂＜801＞POLAROGRAPHY极谱法＜811＞POWDER FINENESS粉剂细度＜821＞RADIOACTIVITY放射性＜823＞POSITRON EMISSION TOMOGRAPHY DRUGS FOR COMPOUNDING, INVESTIGATIONAL, AND RESEARCH USES用于正电子发射断层造影术的放射性药物＜831＞REFRACTIVE INDEX折光率＜841＞SPECIFIC GRAVITY比重＜846＞SPECIFIC SURFACE AREA 比表面积＜851＞SPECTROPHOTOMETRY AND LIGHT-SCATTERING分光光度计与光散射＜852＞ATOMIC ABSORPTION SPECTROSCOPY 原子吸收光谱＜853＞FLUORESCENCE SPECTROSCOPY 荧光光谱＜854＞MID-INFRARED SPECTROSCOPY 中红外光谱＜857＞ULTRAVIOLET-VISIBLE SPECTROSCOPY 紫外可见光谱＜861＞SUTURES—DIAMETER缝线－直径？＜871＞SUTURES—NEEDLE ATTACHMENT缝线－穿孔实验＜881＞TENSILE STRENGTH张力＜891＞THERMAL ANALYSIS热分析＜905＞UNIFORMITY OF DOSAGE UNITS制剂单位的含量均匀度＜911＞VISCOSITY—CAPILLARY METHODS黏度-毛细管法＜912＞VISCOSITY—ROTATIONAL METHODS 黏度-旋转法＜913＞VISCOSITY—ROLLING BALL METHOD 黏度-球法＜921＞W ATER DETERMINATION水分测定＜941＞CHARACTERIZATION OF CRYSTALLINE ANDPARTIALLY CRYSTALLINE SOLIDS BY X-RAY POWDER DIFFRACTION (XRPD)X光衍射General Information通用信息＜1005＞ACOUSTIC EMISSION 声频发射＜1010＞ANALYTICAL DATA—INTERPRETATION AND TREATMENT分析数据－解释与处理＜1015＞AUTOMATED RADIOCHEMICAL SYNTHESIS APPARATUS放射性自动合成装置＜1024＞BOVINE SERUM 牛血清＜1027＞FLOW CYTOMETRY 流式细胞仪＜1030＞BIOLOGICAL ASSAY CHAPTERS—OVERVIEW AND GLOSSARY生物测定章节-综述和术语＜1031＞THE BIOCOMPATIBILITY OF MATERIALS USED IN DRUG CONTAINERS, MEDICAL DEVICES, AND IMPLANTS 用于药物容器、医疗设施和植入剂的材料的生物相容性＜1034＞ANALYSIS OF BIOLOGICAL ASSAYS 生物测定分析＜1035＞BIOLOGICAL INDICATORS FOR STERILIZATION灭菌用生物指示剂＜1041＞BIOLOGICS生物制剂＜1043＞Ancillary Material for Cell, Gene, and Tissue-Engineered Products细胞，基因与组织设计产品的辅助材料＜1044＞CRYOPRESERV ATION OF CELLS 细胞低温保存＜1045＞BIOTECHNOLOGY-DERIVED ARTICLES生物技术提取产品＜1046＞CELLULAR AND TISSUE-BASED PRODUCTS细胞与组织产品＜1047＞GENE THERAPY PRODUCTS 基因治疗产品＜1048＞QUALITY OF BIOTECHNOLOGICAL PRODUCTS: ANALYSIS OF THE EXPRESSION CONSTRUCT IN CELLS USED FOR PRODUCTION OF r-DNA DERIVED PROTEIN PRODUCTS 生物技术产品的质量：从蛋白质产品中提取的r-DNA产品在细胞中表达结构的分析＜1049＞QUALITY OF BIOTECHNOLOGICAL PRODUCTS: STABILITY TESTING OF BIOTECHNOLOGICAL/BIOLOGICAL PRODUCTS生物技术产品的质量：生物技术/生物产品的稳定性实验＜1050＞VIRAL SAFETY EV ALUATION OF BIOTECHNOLOGY PRODUCTS DERIVED FROM CELL LINES OF HUMAN OR ANIMAL ORIGIN从人或动物细胞中提取的生物技术产品的病毒安全性评估＜1051＞CLEANING GLASS APPARATUS玻璃容器的清洗＜1052＞BIOTECHNOLOGY-DERIVED ARTICLES—AMINO ACID ANALYSIS生物技术提取法-氨基酸测定＜1053＞CAPILLARY ELECTROPHORESIS 毛细管电泳法＜1054＞BIOTECHNOLOGY-DERIVED ARTICLES—ISOELECTRIC FOCUSING生物技术提取法-等电点聚集＜1055＞BIOTECHNOLOGY-DERIVED ARTICLES—PEPTIDE MAPPING生物技术提取法-肽谱＜1056＞BIOTECHNOLOGY-DERIVED ARTICLES—POLYACRYLAMIDE GEL ELECTROPHORESIS 生物技术提取法-凝胶电泳＜1057＞BIOTECHNOLOGY-DERIVED ARTICLES—TOTAL PROTEIN ASSAY生物技术提取法-总蛋白测定＜1058＞ANALYTICAL INSTRUMENT QUALIFICATION 分析仪器要求＜1059＞EXCIPIENT PERFORMANCE 赋形剂＜1061＞COLOR—INSTRUMENTAL MEASUREMENT显色－仪器测量＜1065＞Ion Chromatography 离子色谱法＜1066＞PHYSICAL ENVIRONMENTS THAT PROMOTE SAFE MEDICATION USE物理环境促使安全使用药物＜1072＞DISINFECTANTS AND ANTISEPTICS 消毒剂和防腐剂＜1074＞EXCIPIENT BIOLOGICAL SAFETY EV ALUATION GUIDELINES赋形剂（辅料）生物安全性评估指导＜1078＞GOOD MANUFACTURING PRACTICES FOR BULK PHARMACEUTICAL EXCIPIENTS 批药品赋形剂的生产管理规范＜1079＞Good Storage and Shipping Practices 良好的贮存与运输规范＜1080＞BULK PHARMACEUTICAL EXCIPIENTS—CERTIFICATE OF ANALYSIS批药品赋形剂-COA＜1084＞GLYCOPROTEIN AND GLYCAN ANALYSIS—GENERAL CONSIDERATIONS 糖蛋白和多糖分析-一般通则＜1086＞IMPURITIES IN DRUG SUBSTANCES AND DRUG PRODUCTS药物和药物产品中的杂质＜1087＞APPARENT INTRINSIC DISSOLUTION—DISSOLUTION TESTING PROCEDURES FOR ROTATING DISK AND STATIONARY DISK内部的溶出度-旋转和静止溶出检测程序？＜1088＞IN VITRO AND IN VIVO EV ALUATION OF DOSAGEFORMS体内与体外的剂型的评估＜1090＞ASSESSMENT OF DRUG PRODUCT PERFORMANCE-BIOAV AILABILITY, BIOEQUIV ALENCE, AND DISSOLUTION药物产品性能评估：生物利用度、生物等效性和溶出＜1091＞LABELING OF INACTIVE INGREDIENTS非活性成分的标示＜1092＞THE DISSOLUTION PROCEDURE: DEVELOPMENT AND V ALIDATION溶出程序：开发与验证＜1094＞CAPSULES—DISSOLUTION TESTING AND RELATED QUALITY ATTRIBUTES 胶囊-关于产品质量的溶出测定＜1097＞BULK POWDER SAMPLING PROCEDURES：粉末样品取样程序＜1102＞IMMUNOLOGICAL TEST METHODS—GENERAL CONSIDERATIONS免疫测试方法-总则＜1103＞IMMUNOLOGICAL TEST METHODS—ENZYME-LINKED IMMUNOSORBENT ASSAY (ELISA) 免疫学测试方法-酶联免疫吸附测定＜1104＞IMMUNOLOGICAL TEST METHODS—IMMUNOBLOT ANALYSIS免疫测试方法-免疫印迹法＜1105＞IMMUNOLOGICAL TEST METHODS—SURFACE PLASMON RESONANCE 免疫测试方法-表面等离子体共振＜1106＞IMMUNOGENICITY ASSAYS—DESIGN AND VALIDATION OF IMMUNOASSAYS TO DETECT ANTI-DRUG ANTIBODIES＜1111＞MICROBIOLOGICAL EXAMINATION OF NONSTERILE PRODUCTS: ACCEPTANCE CRITERIA FORPHARMACEUTICAL PREPARATIONS AND SUBSTANCES FOR PHARMACEUTICAL USE非无菌产品的微生物学检查：药用制剂和制药过程使用的物质接受标准＜1112＞MICROBIAL CHARACTERIZATION, IDENTIFICATION, AND STRAIN TYPING 非无菌药物产品水活性测定应用＜1113＞MICROBIOLOGICAL ATTRIBUTES OF NONSTERILE PHARMACEUTICAL PRODUCTS 非无菌药品中的微生物分布＜1115＞BIOBURDEN CONTROL OF NONSTERILE DRUG SUBSTANCES AND PRODUCTS 非无菌药物和产品的生物负载控制＜1116＞MICROBIOLOGICAL CONTROL AND MONITORING OF ASEPTIC PROCESSING ENVIRONMENTS洁净的房间与其它可控环境的微生物评估＜1117＞MICROBIOLOGICAL BEST LABORATORY PRACTICES 微生物最优实验室规范＜1118＞MONITORING DEVICES—TIME, TEMPERATURE, AND HUMIDITY监控装置－时间、温度与湿度＜1119＞NEAR-INFRARED SPECTROPHOTOMETRY近红外分光光度测定法＜1120＞Raman Spectrophotometry 拉曼分光光度测定法＜1121＞NOMENCLATURE命名＜1125＞NUCLEIC ACID-BASED TECHNIQUES—GENERAL 核酸技术-通则＜1126＞NUCLEIC ACID-BASED TECHNIQUES—EXTRACTION, DETECTION, AND SEQUENCING 核酸技术-提取、检测、测序＜1127＞NUCLEIC ACID-BASED TECHNIQUES—AMPLIFICATION 核酸技术-扩增＜1128＞NUCLEIC ACID-BASED TECHNIQUES—MICROARRAY 核酸技术-微阵列＜1129＞NUCLEIC ACID-BASED TECHNIQUES—GENOTYPING 核酸技术-基因分型＜1130＞NUCLEIC ACID-BASED TECHNIQUES—APPROACHES FOR DETECTING TRACE NUCLEIC ACIDS (RESIDUAL DNA TESTING)核酸技术-探测微量核酸的应用（残留DNA测试）＜1136＞PACKAGING AND REPACKAGING—SINGLE-UNIT CONTAINERS包装和再包装－单一容器＜1151＞PHARMACEUTICAL DOSAGE FORMS药物剂型＜1152＞ANIMAL DRUGS FOR USE IN ANIMAL FEEDS兽药在动物饲料中的使用＜1160＞PHARMACEUTICAL CALCULATIONS IN PRESCRIPTION COMPOUNDING 按处方混合的药物的计算＜1163＞QUALITY ASSURANCE IN PHARMACEUTICAL COMPOUNDING按处方混合的药物的质量保证＜1171＞PHASE-SOLUBILITY ANALYSIS相溶解分析＜1174＞Powder Flow 粉末流动性＜1176＞PRESCRIPTION BALANCES AND VOLUMETRIC APPARATUS 处方天平与容量器具＜1177＞Good Packaging Practices 良好的包装操作＜1178＞Good Repackaging Practices 良好的再包装操作＜1180＞HUMAN PLASMA 人血浆＜1181＞SCANNING ELECTRON MICROSCOPY扫描电子显微镜＜1184＞SENSITIZATION TESTING 致敏测试＜1191＞STABILITY CONSIDERATIONS IN DISPENSING PRACTICE分装操作中稳定性考察＜1195＞SIGNIFICANT CHANGE GUIDE FOR BULK PHARMACEUTICAL EXCIPIENTS 散装药用辅料更换指导原则＜1197＞GOOD DISTRIBUTION PRACTICES FOR BULK PHARMACEUTICAL EXCIPIENTS 散装药用辅料良好的分装操作＜1207＞STERILE PRODUCT PACKAGING—INTEGRITY EV ALUATION无菌产品包装－完整性评估＜1208＞STERILITY TESTING—V ALIDATION OF ISOLATOR SYSTEMS无菌实验－隔离系统的验证＜1209＞STERILIZATION—CHEMICAL AND PHYSICOCHEMICAL INDICATORS AND INTEGRATORS灭菌－化学与物理化学的指示剂以及二者的综合＜1211＞STERILIZATION AND STERILITY ASSURANCE OF COMPENDIAL ARTICLES 药典物品中的灭菌与灭菌保证＜1216＞TABLET FRIABILITY片剂的脆碎度＜1217＞TABLET BREAKING FORCE 片剂断裂力＜1222＞TERMINALLY STERILIZED PHARMACEUTICAL PRODUCTS—PARAMETRIC RELEASE 药品终端灭菌－放行参数＜1223＞V ALIDATION OF ALTERNATIVE MICROBIOLOGICAL METHODS可供选择的微生物学方法的验证＜1224＞TRANSFER OF ANALYTICAL PROCEDURES 分析方法转移＜1225＞V ALIDATION OF COMPENDIAL PROCEDURES药典方法的验证＜1226＞VERIFICATION OF COMPENDIAL PROCEDURES 药典方法的确认＜1227＞V ALIDATION OF MICROBIAL RECOVERY FROM PHARMACOPEIAL ARTICLES从药物中回收微生物的验证＜1229＞STERILIZATION OF COMPENDIAL ARTICLES 药典灭菌过程＜1229.1＞STEAM STERILIZATION BY DIRECT CONTACT 直接蒸汽灭菌＜1229.2＞MOIST HEAT STERILIZATION OF AQUEOUS LIQUIDS 水溶液的湿热灭菌＜1229.3＞MONITORING OF BIOBURDEN 生物负载监控＜1229.4＞STERILIZING FILTRATION OF LIQUIDS 溶液的无菌过滤器＜1229.6＞LIQUID-PHASE STERILIZATION 液态灭菌＜1229.7＞GASEOUS STERILIZATION 气态灭菌＜1229.8＞DRY HEAT STERILIZATION 干热灭菌＜1229.10＞RADIATION STERILIZATION 辐射灭菌＜1230＞W ATER FOR HEMODIALYSIS APPLICATIONS 血液透析过程用水＜1231＞W ATER FOR PHARMACEUTICAL PURPOSES制药用水＜1234＞VACCINES FOR HUMAN USE—POLYSACCHARIDE AND GLYCOCONJUGATE VACCINES 人用疫苗-多糖和糖复合物疫苗＜1235＞V ACCINES FOR HUMAN USE—GENERAL CONSIDERATIONS 人用疫苗-通则＜1237＞VIROLOGY TEST METHODS 病毒测试方法＜1238＞V ACCINES FOR HUMAN USE—BACTERIAL V ACCINES 人用疫苗-细菌疫苗＜1240＞VIRUS TESTING OF HUMAN PLASMA FOR FURTHER MANUFACTURE下一步使用人血浆的病毒测试＜1241＞W ATER–SOLID INTERACTIONS IN PHARMACEUTICAL SYSTEMS在药物系统中水与固体的相互作用＜1251＞WEIGHING ON AN ANALYTICAL BALANCE关于分析天平的称重＜1265＞Written Prescription Drug Information－Guidelines 书面的处方药信息－指南＜1285＞PREPARATION OF BIOLOGICAL SPECIMENS FOR HISTOLOGIC AND IMMUNOHISTOCHEMICAL ANALYSIS 为了组织和免疫组织分析的生物标本制备＜1285.1＞HEMATOXYLIN AND EOSIN STAINING OF SECTIONED TISSUE FOR MICROSCOPIC EXAMINATION显微镜观察用苏木精和伊红染色的切片＜1601＞PRODUCTS FOR NEBULIZATION—CHARACTERIZATION TESTS 产品雾化状态-性状描述＜1644＞THEORY AND PRACTICE OF ELECTRICAL CONDUCTIVITY MEASUREMENTS OF SOLUTIONS溶液电导值测量方法的理论与实践＜1660＞EV ALUATION OF THE INNER SURFACE DURABILITY OF GLASS CONTAINERS 玻璃容器内表面耐久性评估＜1724＞SEMISOLID DRUG PRODUCTS—PERFORMANCE TESTS 半固态药物产品-性能测试＜1736＞APPLICATIONS OF MASS SPECTROMETRY 质谱应用＜1761＞APPLICATIONS OF NUCLEAR MAGNETIC RESONANCE SPECTROSCOPY核磁共振光谱应用＜1787＞MEASUREMENT OF SUBVISIBLE PARTICULATE MATTER IN THERAPEUTIC PROTEIN INJECTIONS用显微镜测量方法测量治疗性蛋白注射剂的不溶性微粒＜1788＞METHODS FOR THE DETERMINATION OF PARTICULATE MATTER IN INJECTIONS AND OPHTHALMIC SOLUTIONS注射剂和眼用溶液的不溶性微粒测定的方法选择＜1852＞ATOMIC ABSORPTION SPECTROSCOPY—THEORY AND PRACTICE原子吸收光谱-理论与实践＜1853＞FLUORESCENCE SPECTROSCOPY—THEORY AND PRACTICE荧光光谱-理论与实践＜1854＞MID-INFRARED SPECTROSCOPY—THEORY AND PRACTICE中红外光谱-理论与实践＜1857＞ULTRA VIOLET-VISIBLE SPECTROSCOPY—THEORY AND PRACTICE紫外可见光谱-理论与实践＜1911＞RHEOMETRY 流变测定Dietary Supplements营养补充剂General Tests and Assays 一般检查法与测定法＜2021＞MICROBIAL ENUMERATION TESTS—NUTRITIONAL AND DIETARY SUPPLEMENTS…3080微生物数量实验－营养与食品添加剂＜2022＞MICROBIOLOGICAL PROCEDURES FOR ABSENCE OF SPECIFIED MICROORGANISMS—NUTRITIONAL AND DIETARY SUPPLEMENTS (3083)不得检出特定微生物的程序－营养与营养补充剂＜2023>MICROBIOLOGICAL ATTRIBUTES OF NONSTERILE NUTRITIONAL AND DIETARY SUPPLEMENTS……3087非无菌的营养与食品添加剂中的微生物分布<2040>DISINTEGRATION AND DISSOLUTION OF DIETARY SUPPLEMENTS (3089)食品添加剂的崩解与溶出<2091>WEIGHT V ARIATION OF DIETARYSUPPLEMENTS……3092食品添加剂的重量差异<2750>MANUFACTURING PRACTICES FOR DIETARY SUPPLEMENTS (3093)食品添加剂的生产操作。

<711> DISSOLUTION溶出度<USP39-NF34 Page540> General chapter Dissolution <711> is being harmonized with the corresponding texts of the European Pharmacopoeia and/or the Japanese Pharmacopoeia. These pharmacopeias have undertaken to not make any unilateral change to this harmonized chapter.通则<711>溶出度与欧盟药典和日本药典中的相应部分相统一.这三部药典承诺不做单方面的修改.Portions of the present general chapter text that are national USP text, and therefore not part of the harmonized text, are marked with symbols to specify this fact.本章中的部分文字为本国USP内容,并没有与其他药典统一.此部分以〔〕标注.This test is provided to determine pliance with the dissolution requirements where stated in the individual monograph for dosage forms administered orally. In this general chapter, a dosage unit is defined as 1 tablet or 1 capsule or the amount specified. Of the types of apparatus designs described herein, use the one specified in the individual monograph. Where the label states that an article is enteric coated and a dissolution or disintegration test does not specifically state that it is to be applied to delayed-release articles and is included in the individual monograph, the procedure and interpretation given for Delayed-Release Dosage Forms are applied, unless otherwise specified in the individual monograph.本测试用于检测药品口服制剂的溶出度是否符合各论中的规定.本章中,除另有规定外,单位制剂定义为1片或1粒胶囊.对于本章中所述多种仪器,使用各论中规定的种类.除各论中另有规定外,如果检品是肠溶衣片且各论中的溶出度或崩解时限检查项下没有特别指出适用迟释剂的,使用本章中适用于迟释剂的流程和解释.FOR DOSAGE FORMS CONTAINING OR COATED WITH GELATIN涂有或包含明胶的剂型If the dosage form containing gelatin does not meet the criteria in the appropriate Acceptance Table <see Interpretation, Immediate-Release Dosage Forms, Extended-Release Dosage Forms, or Delayed-Release Dosage Forms> because of evidence of the presence of cross-linking, the dissolution procedure should be repeated with the addition of enzymes to the medium, as described below, and the dissolution results should be evaluated starting at the first stage of the appropriate Acceptance Table. It is not necessary to continue testing through the last stage <up to 24 units> when criteria are not met during the first stage testing, and evidence of cross-linking is observed.如果剂型中含有明胶,其不符合验收表中的标准〔见判断,速释制剂,延释制剂,缓释制剂〕,因为存在明胶交联结合作用,它的溶解过程与外加的媒介酶是重复的,见下面的描述,并且溶解结果可以通过适当的验收表的开始的第一阶段标准进行评估.如果溶出结果不满足第一阶段的测试标准,那么就没有必要继续测试到最后阶段,并且也证明了明胶交联结合作用的存在.Gelatin, in the presence of certain pounds and/or in certain storage conditions, including but not restricted to high humidity and temperature, may present cross-linking.A pellicle may form on the external and/or internal surface of the gelatin capsule shell or on the dosage form that prevents the drug from being released during dissolution testing <see more information in Capsules—Dissolution Testing and Related Quality Attributes <1094>>.明胶,存在于某一处方和/或某一储存条件下,如：高温高湿,可能存在明胶交联结合作用.在胶囊壳或其他剂型的外表面和/或内表面形成一层膜阻止溶出试验过程中药物的释放〔见胶囊-溶出度检测和相关质量属性<1094>〕.N OTE— All references to a chapter above <1000> are for information purposes only, for use as a helpful resource. These chapters are not mandatory unless explicitly called out for this application.注-超过<1000>章节的所有引用应用的目的仅为提供参考信息.这些章节是非强制的,除非另有规定.Dissolution Medium with pH ≤4.0 pH≤4.0的溶出介质Enzyme: Pepsin, activity determined by the procedure in purified pepsin, in the Reagent Specifications section酶：胃蛋白酶,活性视试剂规格部分中的胃蛋白酶提纯过程而定.Amount: A quantity of pepsin that results in an activity of NMT 750,000 Units/L of dissolution medium数量：一些胃蛋白酶对溶出介质提供NMT 750,000 单位/L的生物活性. Dissolution Medium with pH >4.0 and <6.8pH >4.0 和<6.8的溶出介质Enzyme: Papain, activity determined by the Assay test in the monograph for Papain; or bromelain, activity determined by the procedure in bromelain, in the Reagent Specifications section酶：木瓜蛋白酶,活性视木瓜蛋白酶专论中的分析测试而定；或菠萝蛋白酶,活性视试剂规格部分中的菠萝蛋白酶生产过程而定.Amount: A quantity of papain that results in an activity of NMT 550,000 Units/L of dissolution medium, or a quantity of bromelain that results in an activity of NMT 30 gelatin-digesting units <GDU>/L of dissolution medium数量：一些木瓜蛋白酶对溶出介质提供NMT 550,000 单位/L的生物活性；一些菠萝蛋白酶对溶出介质提供NMT 30明胶消化单位/L的生物活性.Dissolution Medium with pH ≥6.8pH≥6.8的溶出介质Enzyme: Pancreatin, protease activity determined by the procedure in Assay for protease activity <Casein digestive power> in the monograph for Pancreatin酶：胰液素,蛋白酶活性视胰液素专论中的蛋白酶活性〔酪蛋白消化能力〕分析中的生产过程而定.Amount: A quantity of pancreatin that results in a protease activity of NMT 2000 Units/L of dissolution medium数量：一些胰液素对溶出介质提供NMT 550,000 单位/L的蛋白酶活性. Dissolution Medium Containing Surfactant or Other Ingredients Known to Denature the Enzyme含有表面活性剂或其他已知成分变性酶的溶出介质If the dissolution medium contains surfactant or other ingredients that are known to denature the enzyme used, a pretreatment step in the dissolution testing of the dosage form may be applied. This pretreatment step is done using the specified dissolutionmedium without the surfactant or the ingredient and with the addition of the appropriate amount of enzyme according to the medium pH. The amount of enzyme added is appropriate to the volume of dissolution medium used in the pretreatment. To achieve the specified medium volume for the final dissolution testing, the pretreatment step may be conducted with a smaller volume of medium without the ingredient such that the final volume is obtained when the ingredient is added at the end of the pretreatment step. All of the other conditions of the test <apparatus, rotation, or flow rate> should remain as described in the method or monograph. Typically, the duration of the pretreatment step is NMT 15 min. The required pretreatment time should be evaluated on a case-by-case basis and should be scientifically justified. This time should be included in the total time of the test. As an example, if the total time of the test is 45 min and 15 min are used in the pretreatment step, the test will continue for 30 min after the addition of the ingredient.如果溶出介质中添加了表面活性剂或其他已知成分的变性酶,那么此溶出实验就要把预处理步骤考虑进去.预处理过程就是是根据溶出介质的pH来确定加入酶的量,此处的溶出介质不含有表面活性剂和原料.酶加入的量要适合预处理所用的溶出介质的体积.为了达到最终溶出试验所需要的特定的溶出介质的体积,预处理阶段所用的溶出介质〔不含原料〕的体积要稍微小点,如此在预处理最后阶段加入原料的时候方可获得最终的溶出介质体积.其他所有的测试条件〔如：设备、转速、流速〕应该与方法或专论中描述的一致.通常预处理阶段的持续时间为NMT 15 min.所需的预处理时间应该根据具体案例具体分析,且应该科学、合理.预处理时间应该包含在实验的总时间里.例如,如果实验的总时间为45min,预处理时间为15min,那么加入原料后实验还要继续进行30min.USP Reference Standards 〈11〉—USP Prednisone Tablets RS.USP参考标准<11>-USP强的松片RS.APPARATUS仪器Apparatus 1 <Basket Apparatus>第1法〔篮法〕The assembly consists of the following: a vessel, which may be covered, and made of glass or other inert, transparent material;1 a motor; a metallic drive shaft; and a cylindrical basket. The vessel is partially immersed in a suitable water bath of any convenient size or heated by a suitable device, such as a heating jacket. The water bath or heating device permits holding the temperature inside the vessel at 37 ± 0.5° during the test and keeps the bath fluid in constant, smooth motion. No part of the assembly, including the environment in which the assembly is placed, contributes significant motion, agitation, or vibration beyond that due to the smoothly rotating, stirring element. An apparatus that permits observation of the specimen and of the stirring element during the test is preferable. The vessel is cylindrical, with a hemispherical bottom and with one of the following dimensions and capacities: for a nominal capacity of 1 L, the height is 160–210 mm, and its inside diameter is 98–106 mm; for a nominal capacity of 2 L, the height is 280–300 mm, and its inside diameter is 98–106 mm; and for a nominal capacity of 4 L, the height is 280–300 mm, and its inside diameter is 145–155 mm. Its sides are flanged at the top. A fitted cover may be used to retardevaporation.2 The shaft is positioned so that its axis is NMT 2 mm at any point from the vertical axis of the vessel and rotates smoothly and without significant wobble that could affect the results. A speed-regulating device is used that allows the shaft rotation speed to be selected and maintained at the specified rate given in the individual monograph within ±4%.设备由下列部分组成：有盖或无盖的溶出杯,由玻璃或其他惰性的透明材料1制成；马达；转轴；转篮.溶出杯部分浸没在合适大小的水浴中,或者由合适的装置加热,例如电热套.水浴或加热装置需能在测试过程中将杯内温度保持在37±0.5℃,并且容许杯内液体持续、平缓的流动.整个仪器包括周围的环境,除了平稳转动的搅拌部件,不得有明显的运动,搅动或振动.仪器最好能允许在检测过程中能够观察到检品和搅拌部件.溶出杯为圆柱形,底部为半球形,尺寸和容积如下：名义容积1L的,高160-210mm,内径98-106mm；名义容积2L的,高280-300mm,内径98-106mm；名义容积4L的,高280-300mm,内径145-155mm.内壁顶部有缘.可以使用合适的盖子减缓溶剂蒸发2.转轴与溶出杯的纵轴在任意部位不得相差差过2mm,转动平滑,无明显摇晃以至于影响检测结果.速度调节装置控制转轴的转速,并可维持在各论中规定值的±4%X围内.Shaft and basket ponents of the stirring element are fabricated of stainless steel, type 316, or other inert material, to the specifications shown in Figure 1. A basket having a gold coating of about 0.0001 inch <2.5 µm> thick may be used. A dosage unit is placed in a dry basket at the beginning of each test. The distance between the inside bottom of the vessel and the bottom of the basket is maintained at 25 ± 2 mm during the test.转轴和篮筐组件由316号不锈钢或者其他惰性材料制成,尺寸如图1所示.可使用镀金厚度0.0001英寸〔2.5μm〕的篮筐.开始检测时,将一剂药品至于干燥的篮筐中.在测试过程中,溶出杯底部到篮筐底部的距离应保持在25±2mm.Figure 1. Basket stirring element.图1. 转篮组成Apparatus 2 <Paddle Apparatus>第2法〔桨法〕Use the assembly from Apparatus 1, except that a paddle formed from a blade and a shaft is used as the stirring element. The shaft is positioned so that its axis is NMT 2 mm from the vertical axis of the vessel at any point and rotates smoothly without significant wobble that could affect the results. The vertical center line of the blade passes through the axis of the shaft so that the bottom of the blade is flush with the bottom of the shaft. The paddle conforms to the specifications shown in Figure 2. The distance of 25 ± 2 mm between the bottom of the blade and the inside bottom of the vessel is maintained during the test. The metallic or suitably inert, rigid blade and shaft pose a single entity. A suitable two-part, detachable design may be used, provided that the assembly remains firmly engaged during the test. The paddle blade and shaft may be coated with a suitable coating so as to make both of them inert. The dosage unit is allowed to sink to the bottom of the vessel before rotation of the blade is started. A small, loose piece of nonreactive material, such as NMT a few turns of wire helix, may be attached to dosage units that would otherwise float. An alternative sinker device is shown in Figure 2a. Other validated sinker devices may be used.使用第1法中的设备,除了使用一个由叶片和转轴组成的桨作为搅拌单元.转轴与溶出杯的纵轴在任意部位不得相差差过2mm,转动平滑,无明显摇晃以至于影响检测结果.叶片的垂直中性线穿过转轴的轴线,叶片的下缘与转轴底部平齐.桨的尺寸应符合图2中的规定.在测试过程中,叶片底部与溶出杯底部的距离应保持在25±2mm.金属或硬质的叶片和转轴应是一个整体.两部分组合的设计也可以使用,只要组件在检测过程中牢固固定在一起.可以在桨叶和转轴上涂布合适的涂层以使其为惰性.在桨叶开始旋转前,将一剂药品沉至溶出杯底.如果药剂浮在页面上,可以在其上附着一个惰性,松弛的小部件,例如几圈线圈,使其沉没.图2是一种可替代使用的沉子.其他经验证的沉子也可以使用.Figure 2. Paddle stirring element.图2. 搅拌桨组成Figure 2a. Alternative sinker. All dimensions are expressed in mm.图2a. 可选的沉降篮〔单位均为mm〕Apparatus 3 <Reciprocating Cylinder>第3法〔往复圆筒法〕NOT ACCEPTED BY THE JAPANESE PHARMACOPOEIA日本药典未收录The assembly consists of a set of cylindrical, flat-bottomed glass vessels; a set of glass reciprocating cylinders; inert fittings <stainless steel type 316 or other suitable material>, and screens that are made of suitable nonsorbing and nonreactive material and that are designed to fit the tops and bottoms of the reciprocating cylinders; and a motor and drive assembly to reciprocate the cylinders vertically inside the vessels; if desired, index the reciprocating cylinders horizontally to a different row of vessels. The vessels are partially immersed in a suitable water bath of any convenient size that permits holding the temperature at 37 ± 0.5° during the test. No part of the assembly, including the environment in which the assembly is placed, contributes significant motion, agitation, or vibration beyond that due to the smooth, vertically reciprocating cylinder. A device is used that allows the reciprocation rate to be selected and maintained at the specified dip rate given in the individual monograph within ±5%. An apparatus that permits observation of the specimens and reciprocating cylinders is preferable. The vessels are provided with evaporation caps that remain in place for the duration of the test. The ponents conform to the dimensions shown in Figure 3, unless otherwise specified in the individual monograph.所用设备包含一套圆柱形平底玻璃杯；一套玻璃往复圆筒；惰性配件〔316号不锈钢或其他合适的材质〕；由合适的非吸附,不反应材料制成的筛网,挡在往复圆筒的上下两端；一套马达和传动装置,将圆筒在玻璃杯中垂直往复运动,如果需要,也可以将往复圆筒平行移至另一行玻璃杯中.玻璃杯部分浸没在合适尺寸的水浴中,水浴温度保持在37±0.5℃.仪器的任何部件,以与仪器所处的环境,都不应当引起明显的移动,搅动,振动,除了平滑的垂直往复运动的圆筒.使用设备维持往复速度在各论中所规定值的±5%X围内.仪器最好可以在检测过程中观察到样品和往复圆筒.玻璃杯配有蒸发帽,在检测中一直盖在玻璃杯上.除另有规定外,各部分的尺寸如图3所示.Figure 3. Apparatus 3 <reciprocating cylinder>.图3. 图3 第3法〔往复圆筒法〕设备Apparatus 4 <Flow-Through Cell>第4法〔流通池法〕The assembly consists of a reservoir and a pump for the Dissolution medium; a flow-through cell; and a water bath that maintains the Dissolution medium at 37 ± 0.5°. Use the specified cell size as given in the individual monograph.所用设备包含一个溶出介质的容器和相应的泵,一个流通池和水浴.水浴将溶出介质保持在37±0.5℃.使用各论中规定的尺寸.The pump forces the Dissolution medium upward through the flow-through cell. The pump has a delivery range between 240 and 960 mL/h, with standard flow rates of 4, 8,and 16 mL/min. It must deliver a constant flow <±5% of the nominal flow rate>; the flow profile is sinusoidal with a pulsation of 120 ± 10 pulses/min. A pump without pulsation may also be used. Dissolution test procedures using a flow-through cell must be characterized with respect to rate and any pulsation.泵将溶出介质推动,向上通过流通池.泵的传输能力在240到960mL每小时之间,标准速率为4,8,16mL每分钟.泵的流速必须均匀〔名义流量的±5%以内〕.泵的流量特性曲线应为正弦波,脉冲为每分钟120 ± 10 冲.无脉冲泵也可以使用.使用流通池法的溶出度测试必须对应特定的流速和脉冲.The flow-through cell <see Figure 4 and Figure 5>, of transparent and inert material, is mounted vertically with a filter system <specified in the individual monograph> that prevents escape of undissolved particles from the top of the cell; standard cell diameters are 12 and 22.6 mm; the bottom cone is usually filled with small glass beads of about 1-mm diameter with one bead of about 5 mm, positioned at the apex to protect the fluid entry tube; and a tablet holder <see Figure 4 and Figure 5> is available for positioning of special dosage forms, e.g., inlay tablets. The cell is immersed in a water bath, and the temperature is maintained at 37 ± 0.5°.由透明且惰性材料制成的流通池〔见图4和图5〕垂直安放,配有过滤系统〔在各论中规定〕以防止未溶解的颗粒从流通池顶部逸出.标准的流通池直径为12和22.6mm.底部的锥形通常填有直径约1mm的小玻璃珠,其中一颗约5mm大的玻璃珠置于顶点处,以保护液体输入管.流通池配有药片架〔见图4和图5〕一满足特殊制剂的需要,如泡腾片.流通池浸没在37±0.5℃的水浴中.Figure 4. Apparatus 4: large cell fortablets and capsules <top>; tablet holderfor the large cell <bottom>. <Allmeasurements are expressed in mmunless noted otherwise.>图4.第4法设备,盛装片剂和胶囊的大流通池〔上〕,大药片架〔下〕.〔除另有说明,所有尺寸单位为mm.〕Figure 5. Apparatus 4: small cell fortablets and capsules <top>; tablet holderfor the small cell <bottom>. <Allmeasurements are expressed in mmunless noted otherwise.>图5 第4法设备,盛装片剂和胶囊的小流通池〔上〕,小药片架〔下〕.〔除另有说明,所有尺寸单位为mm.〕The apparatus uses a clamp mechanism and two O-rings to assemble the cell. The pump is separated from the dissolution unit to shield the latter against any vibrations originating from the pump. The position of the pump should not be on a level higher than the reservoir flasks. Tube connections are as short as possible. Use suitably inert tubing, such as polytef, with about a 1.6-mm inner diameter and chemically inert, flanged-end connections.流通池使用一个架子和2个O形圈固定.泵与溶出单元分开,以防止泵的振动干扰到后者.泵的水平位置不得高于溶出介质容器.管线连接尽可能短.使用合适的惰性管线,如聚四氟乙烯,内径1.6mm.法兰连接也应为化学惰性.APPARATUS SUITABILITY设备适用性The determination of suitability of a test assembly to perform dissolution testing must include conformance to the dimensions and tolerances of the apparatus as given above. In addition, critical test parameters that have to be monitored periodically during use include volume and temperature of the Dissolution medium, rotation speed <Apparatus 1 and Apparatus 2>, dip rate <Apparatus 3>, and flow rate of medium <Apparatus 4>. 溶出度测试仪器的适用性必须包括与上述各仪器在尺寸和限度上的一致性.另外,必须在使用过程中定期观测的关键测试参数包括：溶出介质的温度和体积,转速〔第1法和第2法〕,浸没频率〔第3法〕和溶出介质流速〔第4法〕. Determine the acceptable performance of the dissolution test assembly periodically.The suitability for the individual apparatus is demonstrated by the Performance verification test.定期检测溶出度测试设备的性能.单个设备的适用性由性能验证测试给出. Performance verification test, Apparatus 1 and Apparatus 2: Test USP Prednisone Tablets RS according to the operating conditions specified. The apparatus is suitable if the results obtained are within the acceptable range stated in the technical data sheet specific to the lot used and the apparatus tested.性能验证测试,第1法和第2法：根据规定的操作条件测试USP强的松片RS.如果结果在技术数据表上该批次和所用仪器的的可接受X围内,则设备是适用的. Performance verification test, Apparatus 3: [To e.]性能验证测试,第3法——[待续]Performance verification test, Apparatus 4: [To e.]性能验证测试,第4法——[待续]PROCEDURE测试方法Apparatus 1 and Apparatus 2第1法和第2法IMMEDIATE-RELEASE DOSAGE FORMS速释制剂Place the stated volume of the Dissolution medium <±1%> in the vessel of the specified apparatus given in the individual monograph, assemble the apparatus, equilibrate the Dissolution medium to 37 ± 0.5°, and remove the thermometer. Place 1 dosage unit in the apparatus, taking care to exclude air bubbles from the surface of the dosage unit, and immediately operate the apparatus at the specified rate given in the individual monograph. Within the time interval specified, or at each of the times stated, withdraw a specimen from a zone midway between the surface of the Dissolution medium and the top of the rotating basket or blade, NLT 1 cm from thevessel wall. [N OTE— Where multiple sampling times are specified, replace the aliquots withdrawn for analysis with equal volumes of fresh Dissolution medium at 37°or, where it can be shown that replacement of the medium is not necessary, correct for the volume change in the calculation. Keep the vessel covered for the duration of the test, and verify the temperature of the mixture under test at suitable times. ] Perform the analysis as directed in the individual monograph using a suitable assay method.3 Repeat the test with additional dosage form units.将各论中给出的溶出介质量〔±1%〕加入到规定的容器中,组装好设备,平衡溶出介质温度在37±0.5℃,移出温度计.将1单位剂量的药品小心加入设备中,注意避免表面产生气泡.立即按照各论中规定的速率开动设备.在规定的时间间隔或给定的时间点,从溶出介质液面以下和溶出篮或桨叶顶端之间,离杯壁至少1cm 的区域取出一份试样.[注：如果规定有多次取样,以等体积的37℃溶出介质补偿所取液体.或者,如果有证明不需要补偿介质,在计算中修正溶液体积的变化.在检测中保持容器加盖,并以适当的频率验证溶液的温度.]按照各论中规定的合适的方法进行分析3.重复试验以测试更多的剂量单元.If automated equipment is used for sampling or the apparatus is otherwise modified, verification that the modified apparatus will produce results equivalent to those obtained with the standard apparatus described in this general chapter is necessary.如果使用自动化装置取样或者设备在其他方面做出了更改,需要进行验证以显示修改后的设备可以给出与通用章节中的标准设备等效的结果.Dissolution medium: A suitable dissolution medium is used. Use the solvent specified in the individual monograph. The volume specified refers to measurements made between 20°and 25°. If the Dissolution medium is a buffered solution, adjust the solution so that its pH is within 0.05 unit of the specified pH given in the individual monograph. [ N OTE— Dissolved gases can cause bubbles to form, which may change the results of the test. If dissolved gases influence the dissolution results, dissolved gases should be removed before testing.4 ]溶出介质：使用合适的溶出介质.使用各论中规定的溶剂.所规定的体积指在20和25℃之间所测的值.如果溶出介质是缓冲液,调整缓冲液以保证缓冲液的pH值在各论中规定的pH值的0.05以内.[注：溶解的气体可以导致气泡的生成,从而改变测试结果.如果溶解的气体会影响溶出结果,在测试前除去溶解的气体4.] Time: Where a single time specification is given, the test may be concluded in a shorter period if the requirement for the minimum amount dissolved is met. Specimens are to be withdrawn only at the stated times, within a tolerance of ±2%.时间：当规定了单一的时间时,如果最小溶出量已达到,测试可以提前结束.试样必须在所述时间的±2%X围内取出.Procedure for a pooled sample for immediate-release dosage forms: Use this procedure where Procedure for a Pooled Sample is specified in the individual monograph. Proceed as directed for Immediate-Release Dosage Forms in Apparatus 1 and Apparatus 2 in the Procedure section. bine equal volumes of the filtered solutions of the six or twelve individual specimens withdrawn, and use the pooled sample as the test specimen. Determine the average amount of the active ingredient dissolved in the pooled sample.速释制剂集合样品测试方法：如果各论中有规定测试集合样品,使用本方法.按照测试方法章节中速释制剂第1法和第2法进行.集中全部所测的6或12个单独物种的等体积的溶剂,过滤,使用集合样品作为被测物种,测定集合样品中各活性成分的平均溶出量.EXTENDED-RELEASE DOSAGE FORMS缓释制剂Proceed as directed for Immediate-Release Dosage Forms.按照速释制剂的方法进行.Dissolution medium: Proceed as directed for Immediate-Release Dosage Forms.溶出介质：按照立即释放制剂的方法进行.Time: The test-time points, generally three, are expressed in hours.时间：测试时间点,通常是3个,以小时为单位.DELAYED-RELEASE DOSAGE FORMS NOT ACCEPTED BY THE JAPANESE PHARMACOPOEIA 日本药典未收录的迟释制剂Use Method A or Method B and the apparatus specified in the individual monograph. All test times stated are to be observed within a tolerance of ±2%, unless otherwise specified.按照各论中的规定,使用方法A或方法B.除另有规定外,所有测试时间与规定相差不得过±2%.Method A Procedure <unless otherwise directed in the individual monograph>方法A程序〔除各论中另有规定外〕ACID STAGE酸阶段Place 750 mL of 0.1 N hydrochloric acid in the vessel, and assemble the apparatus. Allow the medium to equilibrate to a temperature of 37 ± 0.5°. Place 1 dosage unit in the apparatus, cover the vessel, and operate the apparatus at the specified rate given in the monograph.向容器中加入0.1N的盐酸750mL,组装设备.将介质平衡在37±0.5℃.将1单位剂量的药品加入设备中,盖上容器,依照各论中规定的速率启动设备.After 2 h of operation in 0.1 N hydrochloric acid, withdraw an aliquot of the fluid, and proceed immediately as directed in the Buffer Stage.在0.1N的盐酸中搅拌2小时后,吸取一份试样溶液,然后立即按照缓冲液阶段的说明继续操作.Perform an analysis of the aliquot using a suitable assay method. The procedure is specified in the individual monograph.以适合的方法测试试样.测试方法在各论中给出.BUFFER STAGE缓冲液阶段[ N OTE— plete the operations of adding the buffer and adjusting the pH within 5 min. ] With the apparatus operating at the rate specified in the monograph, add to the fluid in the vessel 250 mL of 0.20 M tribasic sodium phosphate that has been equilibrated to 37 ± 0.5°. Adjust, if necessary, with 2 N hydrochloric acid or 2 N sodium hydroxide to a pH of 6.8 ± 0.05. Continue to operate the apparatus for 45 min, or for the specified time given in the individual monograph. At the end of the time period, withdraw an aliquot of the fluid, and perform the analysis using a suitable assay method. The procedure is specified in the individual monograph. The test may beconcluded in a shorter time period than that specified for the Buffer Stage if the requirement for the minimum amount dissolved is met at an earlier time.[注：加入缓冲液和调节pH的操作应在5分钟内完成.]设备在各论中规定的速率下运行,向容器中加入250mL预先平衡在37±0.5℃的0.20M的磷酸钠.必要时用2N的盐酸或2N的氢氧化钠调节pH至6.8±0.05.继续运转45分钟或各论中给定的时间.到时间后,吸取一份试样溶液,以适合的方法测试.测试方法在各论中给出.如果缓冲液阶段的最小溶出量已提前达到,测试可以提前结束.Method B Procedure <unless otherwise directed in the individual monograph>方法B程序〔除各论中另有规定外〕ACID STAGE酸阶段Place 1000 mL of 0.1 N hydrochloric acid in the vessel, and assemble the apparatus. Allow the medium to equilibrate to a temperature of 37 ± 0.5°. Place 1 dosage unit in the apparatus, cover the vessel, and operate the apparatus at the rate specified in the monograph. After 2 h of operation in 0.1 N hydrochloric acid, withdraw an aliquot of the fluid, and proceed immediately as directed in the Buffer Stage.向容器中加入0.1N的盐酸1000mL,组装设备.将介质平衡在37±0.5℃.将1单位剂量的药品加入设备中,盖上容器,依照各论中规定的速率启动设备.在0.1N 的盐酸中搅拌2小时后,吸取一份试样溶液,然后立即按照缓冲液阶段的说明继续操作.Perform an analysis of the aliquot using a suitable assay method. The procedure is specified in the individual monograph.以适合的方法测试试样.测试方法在各论中给出.BUFFER STAGE缓冲液阶段[ N OTE— For this stage of the procedure, use buffer that previously has been equilibrated to a temperature of 37 ± 0.5°. ] Drain the acid from the vessel, and add to the vessel 1000 mL of pH 6.8 phosphate buffer, prepared by mixing 0.1 N hydrochloric acid with 0.20 M tribasic sodium phosphate <3:1> and adjusting, if necessary, with 2 N hydrochloric acid or 2 N sodium hydroxide to a pH of 6.8 ± 0.05. [N OTE— This may also be acplished by removing from the apparatus the vessel containing the acid, then replacing it with another vessel containing the buffer, and transferring the dosage unit to the vessel containing the buffer. ][注：此阶段使用预先平衡在37±0.5℃的缓冲液.]抽干容器中的酸液,加入1000mL pH6.8的磷酸盐缓冲液〔0.1N盐酸加0.20M磷酸钠,3：1〕.必要时用2N 的盐酸或2N的氢氧化钠调节pH至6.8±0.05.[注：也可以将设备中盛装酸液的容器移出,换以另一盛装缓冲液的容器,将药剂转移到缓冲液容器中.]Continue to operate the apparatus for 45 min, or for the specified time given in the individual monograph. At the end of the time period, withdraw an aliquot of the fluid, and perform the analysis using a suitable assay method. The procedure is specified in the individual monograph. The test may be concluded in a shorter time period than that specified for the Buffer Stage if the requirement for minimum amount dissolved is met at an earlier time.继续运转45分钟或各论中给定的时间.到时间后,吸取一份试样溶液,以适合的方法测试.测试方法在各论中给出.如果缓冲液阶段的最小溶出量已提前达到,测试可以提前结束.Apparatus 3 <Reciprocating Cylinder>第3法〔往复圆筒法〕NOT ACCEPTED BY THE JAPANESE PHARMACOPOEIA IMMEDIATE-RELEASE DOSAGE FORMS 日本药典未收录的速释制剂Place the stated volume of the Dissolution medium in each vessel of the apparatus, assemble the apparatus, equilibrate the Dissolution medium to 37 ± 0.5°, and remove the thermometer. Place 1 dosage form unit in each of the six reciprocating cylinders, taking care to exclude air bubbles from the surface of each dosage unit, and immediately operate the apparatus as specified in the individual monograph. During the upward and downward strokes, the reciprocating cylinder moves through a total distance of 9.9–10.1 cm. Within the time interval specified, or at each of the times stated, raise the reciprocating cylinders and withdraw a portion of the solution under test from a zone midway between the surface of the Dissolution medium and the bottom of each vessel. Perform the analysis as directed in the individual monograph. If necessary, repeat the test with additional dosage-form units.将指定量的溶出介质加入到设备的每个容器中,组装好设备,平衡溶出介质温度在37±0.5℃,移出温度计.在6个往复圆筒中分别加入1单位剂量的药品,注意避免表面产生气泡.立即按照各论中规定的速率开动设备.在上行和下行冲程中,往复圆筒移动的总距离为9.9到10.1cm.在规定的时间间隔或者每个给定的时间点,抬起往复圆筒,从溶出介质的表面到容器底部的中点区域取出一部分测试溶液.按照各论中的规定测试.必要时重复测试更多份的样品.Dissolution medium: Proceed as directed for Immediate-Release Dosage Forms in Apparatus 1 and Apparatus 2.溶出介质：同第1法和第2法下立即释放制剂项下处理.Time: Proceed as directed for Immediate-Release Dosage Forms in Apparatus 1 and Apparatus 2.时间：同第1法和第2法下立即释放制剂项下处理.EXTENDED-RELEASE DOSAGE FORMS缓释制剂Proceed as directed for Immediate-Release Dosage Forms in Apparatus 3.同第3法下速释制剂项下处理.Dissolution medium: Proceed as directed for Extended-Release Dosage Forms in Apparatus 1 and Apparatus 2.溶出介质：同第1法和第2法下缓释制剂项下处理.Time: Proceed as directed for Extended-Release Dosage Forms in Apparatus 1 and Apparatus 2.时间：同第1法和第2法下缓释制剂项下处理.DELAYED-RELEASE DOSAGE FORMS迟释制剂Proceed as directed for Delayed-Release Dosage Forms, Method B in Apparatus 1 and Apparatus 2, using one row of vessels for the acid stage media and the following row of vessels for the buffer stage media, and using the volume of medium specified <usually 300 mL>.同第1法和第2法下迟释制剂方法B项下处理.酸性阶段使用一排容器,缓冲液阶段使用另一排容器.使用规定体积的介质〔通常为300mL〕.Time: Proceed as directed for Immediate-Release Dosage Forms in Apparatus 1 and Apparatus 2.。

USP38-通用章节指导目录(附录)Guide to General Chapters 通用章节指导General Requirements for Test and Assays检查与含量分析的一般要求＜1＞INJECTIONS AND IMPLANTED DRUG PRODUCTS (PARENTERALS)—PRODUCT QUALITY TESTS 注射和植入药物产品(注射用) —产品质量测试＜1＞INJECTIONS注射剂＜2＞ORAL DRUG PRODUCTS—PRODUCT QUALITY TESTS 口服药物产品质量测试＜3＞TOPICAL AND TRANSDERMAL DRUG PRODUCTS—PRODUCT QUALITY TESTS 局部和透皮药物产品—产品质量测试＜4＞MUCOSAL DRUG PRODUCTS—PRODUCT QUALITY TESTS 粘膜药物产品质量测试＜5＞INHALATION AND NASAL DRUG PRODUCTS—GENERAL INFORMATION AND PRODUCT QUALITY TESTS 吸入剂产品—产品质量测试＜7＞LABELING 标签＜11＞USP REFERENCE STANDARDS USP标准品Apparatus for Test and Assays用于检查与含量分析的器具＜17＞PRESCRIPTION CONTAINER LABELING处方容器标签＜21＞THERMOMETERS温度计＜31＞VOLUMETRIC APPARATUS容量器具＜41＞BALANCES天平Microbiological Tests 微生物检查法＜51＞ANTIMICROBIAL EFFECTIVENESS TESTING抗菌剂有效性检查法＜55＞BIOLOGICAL INDICATORS—RESISTANCE PERFORMANCE TESTS生物指示剂－耐药性实验＜61＞MICROBIOLOGICAL EXAMINATION OF NONSTERILE PRODUCTS: MICROBIAL ENUMERATION TESTS非无菌产品的微生物限度检查：微生物列举检查法＜62＞MICROBIOLOGICAL EXAMINATION OF NONSTERILE PRODUCTS: TESTS FOR SPECIFIED MICROORGANISMS 非无菌产品的微生物限度检查：特定微生物检查法＜63＞MYCOPLASMA TESTS 支原体检查法＜71＞STERILITY TESTS无菌检查法Biological tests and assays生物检查法与测定法＜81＞ANTIBIOTICS—MICROBIAL ASSAYS抗生素－微生物测定＜85＞BACTERIAL ENDOTOXINS TEST细菌内毒素检查法＜87＞BIOLOGICAL REACTIVITY TESTS, IN VITRO体外的生物反应性检查法＜88＞BIOLOGICAL REACTIVITY TESTS, IN VIVO 体内的生物反应性检查法＜89＞ENZYMES USED AS ANCILLARY MATERIALS IN PHARMACEUTICAL MANUFACTURING 药品生产中酶作为辅料所使用＜90＞FETAL BOVINE SERUM—QUALITY ATTRIBUTES AND FUNCTIONALITY TESTS 牛胎儿血清-质量品质和功能检查法＜91＞CALCIUM PANTOTHENATE ASSAY泛酸钙测定法＜92＞GROWTH FACTORS AND CYTOKINES USED IN CELL THERAPY MANUFACTURING 在细胞疗法中使用生长因子和细胞因子＜111＞DESIGN AND ANALYSIS OF BIOLOGICAL ASSAYS 生物测定法的设计与分析＜115＞DEXPANTHENOL ASSAY右泛醇（拟胆碱药）测定法＜121＞INSULIN ASSAYS胰岛素测定法＜121.1＞PHYSICOCHEMICAL ANALYTICAL PROCEDURES FOR INSULINS胰岛素的物理化学分析程序＜123＞GLUCAGON BIOIDENTITY TESTS 高血糖素的生物鉴别检查法＜124＞ERYTHROPOIETIN BIOASSAYS 红细胞生成素的微生物测定＜126＞SOMATROPIN BIOIDENTITY TESTS 生长激素的生物鉴别检查法＜130＞PROTEIN A QUALITY ATTRIBUTES 蛋白质A的质量特征＜151＞PYROGEN TEST热原检查法＜161＞TRANSFUSION AND INFUSION ASSEMBLIES AND SIMILAR MEDICAL DEVICES 输血输液用具以及相类似的医疗器械＜171＞VITAMIN B12 ACTIVITY ASSAY……2548维生素B12活性测定法Chemical Tests and assays化学实验检查与测定法鉴别检查＜181＞IDENTIFICATION—ORGANIC NITROGENOUS BASES鉴别－有机氮碱化合物＜191＞IDENTIFICATION TESTS—GENERAL鉴别实验－通用＜193＞IDENTIFICATION—TETRACYCLINES鉴别－四环素类＜197＞SPECTROPHOTOMETRIC IDENTIFICATION TESTS分光光度计鉴别实验＜201＞THIN-LAYER CHROMATOGRAPHIC IDENTIFICATION TEST薄层色谱鉴别实验Limit Tests 限度检查法＜206＞ALUMINUM铝＜207＞TEST FOR 1,6-ANHYDRO DERIV ATIVE FOR ENOXAPARIN SODIUM依诺肝素钠的酐类衍生物实验＜208＞ANTI-FACTOR Xa AND ANTI-FACTOR IIa ASSAYS FOR UNFRACTIONATED AND LOW MOLECULAR WEIGHT HEPARINS普通肝素和低分子肝素产品中抗体Xa和抗体IIa测定＜209＞LOW MOLECULAR WEIGHT HEPARIN MOLECULAR WEIGHT DETERMINATIONS 低分子肝素钠分子量测定＜211＞ARSENIC砷＜221＞CHLORIDE AND SULFATE氯和硫＜223＞DIMETHYLANILINE二甲基苯胺＜226＞4-EPIANHYDRO-TETRACYCLINE4－？－四环素＜227＞4-AMINOPHENOL IN ACETAMINOPHEN-CONTAINING DRUG PRODUCTS 对乙酰氨酚药物产品中氨基酚＜228＞ETHYLENE OXIDE AND DIOXANE 环氧乙烷和二氧六环＜231＞HEA VY METALS重金属（删除）＜232＞ELEMENTAL IMPURITIES—LIMITS 元素杂质-限度＜233＞ELEMENTAL IMPURITIES—PROCEDURES 元素杂质-规程＜241＞IRON铁＜251＞LEAD铅＜261＞MERCURY汞＜267＞POROSIMETRY BY MERCURY INTRUSION 水银孔隙仪＜268＞POROSITY BY NITROGEN ADSORPTION–DESORPTION 氮吸附-解吸测定孔隙率＜271＞READILY CARBONIZABLE SUBSTANCES TEST易碳化物检查法＜281＞RESIDUE ON IGNITION炽灼残渣＜291＞SELENIUM硒Other Tests and Assays 其它检查法与测定法＜301＞ACID-NEUTRALIZING CAPACITY酸中和容量＜311＞ALGINATES ASSAY藻酸盐测定法＜341＞ANTIMICROBIAL AGENTS—CONTENT 抗菌剂－含量＜345＞Assay for Citric Acid/Citrate and Phosphate 柠檬酸/柠檬酸盐和磷酸盐的测定＜351＞ASSAY FOR STEROIDS类固醇（甾类化合物）测定法＜361> BARBITURATE ASSAY 巴比妥类药物测定法＜371＞COBALAMIN RADIOTRACER ASSAY钴铵素放射性跟踪剂测定法＜381＞ELASTOMERIC CLOSURES FOR INJECTIONS 注射剂的弹性密封件＜391＞EPINEPHRINE ASSAY肾上腺素测定法＜401＞FATS AND FIXED OILS脂肪与混合油＜411＞FOLIC ACID ASSAY叶酸测定法＜413＞IMPURITIES TESTING IN MEDICAL GASES 医用气体杂质检查＜415＞MEDICAL GASES ASSAY 医用气体含量检查＜425＞IODOMETRIC ASSAY—ANTIBIOTICS碘量检查法－抗生素＜429＞LIGHT DIFFRACTION MEASUREMENT OF PARTICLE SIZE粒径的光衍射测量法＜431＞METHOXY DETERMINATION甲氧基测定法＜441＞NIACIN OR NIACINAMIDE ASSAY 烟酰或烟酰胺测定法＜451＞NITRITE TITRATION亚硝酸盐滴定＜461＞NITROGEN DETERMINATION氮测定法＜466＞ORDINARY IMPURITIES一般杂质＜467＞RESIDUAL SOLVENTS残留溶剂＜469＞ETHYLENE GLYCOL, DIETHYLENE GLYCOL, AND TRIETHYLENE GLYCOL IN ETHOXYLATED SUBSTANCES乙氧基物质中乙二醇、二甘醇、三甘醇测定＜471＞OXYGEN FLASK COMBUSTION氧瓶燃烧法＜481＞RIBOFLAVIN ASSAY核黄素（维生素B2）测定法＜501＞SALTS OF ORGANIC NITROGENOUS BASES有机氮盐＜503＞ACETIC ACID IN PEPTIDES 多肽类中乙酸测定＜511＞SINGLE-STEROID ASSAY单一的类固醇测定法＜525＞SULFUR DIOXIDE 二氧化硫＜531＞THIAMINE ASSAY硫胺素测定法＜541＞TITRIMETRY滴定法＜551＞VITAMIN E ASSAY维生素E测定法＜561＞ARTICLES OF BOTANICAL ORIGIN植物起源的药品＜563＞IDENTIFICATION OF ARTICLES OF BOTANICAL ORIGIN植物药品的鉴别＜565＞BOTANICAL EXTRACTS植物提取＜571＞VITAMIN A ASSAY维生素A测定法＜581＞VITAMIN D ASSAY维生素D测定法＜591＞ZINC DETERMINATION锌的测定法Physical Test and Determinations物理检查与测定法＜601＞INHALATION AND NASAL DRUG PRODUCTS: AEROSOLS, SPRAYS, AND POWDERS—PERFORMANCE QUALITY TESTS吸入剂、鼻雾剂：气溶胶，喷雾，干粉-质量通则＜602＞PROPELLANTS 推进剂＜603＞TOPICAL AEROSOLS 局部喷雾剂＜604＞LEAK RATE 渗漏率＜610＞ALTERNATIVE MICROBIOLOGICAL SAMPLING METHODS FOR NONSTERILE INHALED AND NASAL PRODUCTS非无菌吸入和鼻雾剂可供选择的微生物取样方法＜611＞ALCOHOL DETERMINATION乙醇测定法＜616＞BULK DENSITY AND TAPPED DENSITY堆密度与振实密度＜621＞CHROMATOGRAPHY色谱法＜631＞COLOR AND ACHROMICITY呈色与消色＜641＞COMPLETENESS OF SOLUTION溶解度＜643＞TOTAL ORGANIC CARBON总有机碳＜645＞W ATER CONDUCTIVITY水电导率＜651＞CONGEALING TEMPERATURE凝点温度＜659＞PACKAGING AND STORAGE REQUIREMENTS 包装和储藏要求＜660＞CONTAINERS—GLASS 容器-玻璃＜661＞CONTAINERS—PLASTICS容器-塑料＜670＞AUXILIARY PACKAGING COMPONENTS 辅助包装部件＜671＞CONTAINERS—PERFORMANCE TESTING容器－性能测试＜691＞COTTON棉花＜695＞CRYSTALLINITY结晶度＜696＞CHARACTERIZATION OF CRYSTALLINE SOLIDS BY MICROCALORIMETRY AND SOLUTION CALORIMETRY 通过溶液量热学测定结晶性＜697＞CONTAINER CONTENT FOR INJECTIONS 注射剂容器容积＜698＞DELIVERABLE VOLUME抽取体积＜699＞DENSITY OF SOLIDS固体密度＜701＞DISINTEGRATION崩解时限＜705＞QUALITY ATTRIBUTES OF TABLETS LABELED AS HA VING A FUNCTIONAL SCORE ？＜711＞DISSOLUTION 溶出度＜721＞DISTILLING RANGE馏程＜724＞DRUG RELEASE药物释放度＜729＞GLOBULE SIZE DISTRIBUTION IN LIPID INJECTABLE EMULSIONS脂类可注射的乳剂的粒径分布＜730＞Plasma Spectrochemistry 血浆光谱化学？＜731＞LOSS ON DRYING4干燥失重＜733＞LOSS ON IGNITION灼烧失重＜735＞X-RAY FLUORESCENCE SPECTROMETRY X射线光谱＜736＞MASS SPECTROMETRY 质谱＜741＞MELTING RANGE OR TEMPERATURE熔距或熔点＜751＞METAL PARTICLES IN OPHTHALMIC OINTMENTS眼用软膏中的金属粒子＜755＞MINIMUM FILL最低装量＜761＞NUCLEAR MAGNETIC RESONANCE核磁共振＜771＞OPHTHALMIC OINTMENTS眼用软膏＜776＞OPTICAL MICROSCOPY光学显微镜＜781＞OPTICAL ROTATION旋光度＜785＞OSMOLALITY AND OSMOLARITY渗透压＜786＞PARTICLE SIZE DISTRIBUTION ESTIMATION BY ANALYTICAL SIEVING 筛分法估算粒径分布＜787＞SUBVISIBLE PARTICULATE MATTER IN THERAPEUTIC PROTEIN INJECTIONS显微计数法在治疗性蛋白注射剂中应用＜788＞PARTICULATE MATTER IN INJECTIONS注射剂中的不溶性微粒＜789＞PARTICULATE MATTER IN OPHTHALMIC SOLUTIONS眼用溶液中的不溶性微粒＜790＞VISIBLE PARTICULATES IN INJECTIONS 注射剂中可见异物＜791＞pH＜795＞PHARMACEUTICAL COMPOUNDING—NONSTERILE PREPARATIONS药物混合－非无菌制剂＜797＞PHARMACEUTICAL COMPOUNDING—STERILE PREPARATIONS药物混合－无菌制剂＜801＞POLAROGRAPHY极谱法＜811＞POWDER FINENESS粉剂细度＜821＞RADIOACTIVITY放射性＜823＞POSITRON EMISSION TOMOGRAPHY DRUGS FOR COMPOUNDING, INVESTIGATIONAL, AND RESEARCH USES用于正电子发射断层造影术的放射性药物＜831＞REFRACTIVE INDEX折光率＜841＞SPECIFIC GRAVITY比重＜846＞SPECIFIC SURFACE AREA 比表面积＜851＞SPECTROPHOTOMETRY AND LIGHT-SCATTERING分光光度计与光散射＜852＞ATOMIC ABSORPTION SPECTROSCOPY 原子吸收光谱＜853＞FLUORESCENCE SPECTROSCOPY 荧光光谱＜854＞MID-INFRARED SPECTROSCOPY 中红外光谱＜857＞ULTRAVIOLET-VISIBLE SPECTROSCOPY 紫外可见光谱＜861＞SUTURES—DIAMETER缝线－直径？＜871＞SUTURES—NEEDLE ATTACHMENT缝线－穿孔实验＜881＞TENSILE STRENGTH张力＜891＞THERMAL ANALYSIS热分析＜905＞UNIFORMITY OF DOSAGE UNITS制剂单位的含量均匀度＜911＞VISCOSITY—CAPILLARY METHODS黏度-毛细管法＜912＞VISCOSITY—ROTATIONAL METHODS 黏度-旋转法＜913＞VISCOSITY—ROLLING BALL METHOD 黏度-球法＜921＞W ATER DETERMINATION水分测定＜941＞CHARACTERIZATION OF CRYSTALLINE AND PARTIALLY CRYSTALLINE SOLIDS BY X-RAY POWDER DIFFRACTION (XRPD)X光衍射General Information通用信息＜1005＞ACOUSTIC EMISSION 声频发射＜1010＞ANALYTICAL DATA—INTERPRETATION AND TREATMENT分析数据－解释与处理＜1015＞AUTOMATED RADIOCHEMICAL SYNTHESIS APPARATUS放射性自动合成装置＜1024＞BOVINE SERUM 牛血清＜1027＞FLOW CYTOMETRY 流式细胞仪＜1030＞BIOLOGICAL ASSAY CHAPTERS—OVERVIEW AND GLOSSARY生物测定章节-综述和术语＜1031＞THE BIOCOMPATIBILITY OF MATERIALS USED IN DRUG CONTAINERS, MEDICAL DEVICES, AND IMPLANTS用于药物容器、医疗设施和植入剂的材料的生物相容性＜1034＞ANALYSIS OF BIOLOGICAL ASSAYS 生物测定分析＜1035＞BIOLOGICAL INDICATORS FOR STERILIZATION灭菌用生物指示剂＜1041＞BIOLOGICS生物制剂＜1043＞Ancillary Material for Cell, Gene, and Tissue-Engineered Products细胞，基因与组织设计产品的辅助材料＜1044＞CRYOPRESERV ATION OF CELLS 细胞低温保存＜1045＞BIOTECHNOLOGY-DERIVED ARTICLES生物技术提取产品＜1046＞CELLULAR AND TISSUE-BASED PRODUCTS细胞与组织产品＜1047＞GENE THERAPY PRODUCTS 基因治疗产品＜1048＞QUALITY OF BIOTECHNOLOGICAL PRODUCTS: ANALYSIS OF THE EXPRESSION CONSTRUCT IN CELLS USED FOR PRODUCTION OF r-DNA DERIVED PROTEIN PRODUCTS 生物技术产品的质量：从蛋白质产品中提取的r-DNA产品在细胞中表达结构的分析＜1049＞QUALITY OF BIOTECHNOLOGICAL PRODUCTS: STABILITY TESTING OF BIOTECHNOLOGICAL/BIOLOGICAL PRODUCTS生物技术产品的质量：生物技术/生物产品的稳定性实验＜1050＞VIRAL SAFETY EV ALUATION OF BIOTECHNOLOGY PRODUCTS DERIVED FROM CELL LINES OF HUMAN OR ANIMAL ORIGIN从人或动物细胞中提取的生物技术产品的病毒安全性评估＜1051＞CLEANING GLASS APPARATUS玻璃容器的清洗＜1052＞BIOTECHNOLOGY-DERIVED ARTICLES—AMINO ACID ANALYSIS生物技术提取法-氨基酸测定＜1053＞CAPILLARY ELECTROPHORESIS 毛细管电泳法＜1054＞BIOTECHNOLOGY-DERIVED ARTICLES—ISOELECTRIC FOCUSING生物技术提取法-等电点聚集＜1055＞BIOTECHNOLOGY-DERIVED ARTICLES—PEPTIDE MAPPING生物技术提取法-肽谱＜1056＞BIOTECHNOLOGY-DERIVED ARTICLES—POLYACRYLAMIDE GEL ELECTROPHORESIS 生物技术提取法-凝胶电泳＜1057＞BIOTECHNOLOGY-DERIVED ARTICLES—TOTAL PROTEIN ASSAY生物技术提取法-总蛋白测定＜1058＞ANALYTICAL INSTRUMENT QUALIFICATION 分析仪器要求＜1059＞EXCIPIENT PERFORMANCE 赋形剂＜1061＞COLOR—INSTRUMENTAL MEASUREMENT显色－仪器测量＜1065＞Ion Chromatography 离子色谱法＜1066＞PHYSICAL ENVIRONMENTS THAT PROMOTE SAFE MEDICATION USE物理环境促使安全使用药物＜1072＞DISINFECTANTS AND ANTISEPTICS 消毒剂和防腐剂＜1074＞EXCIPIENT BIOLOGICAL SAFETY EV ALUATION GUIDELINES赋形剂（辅料）生物安全性评估指导＜1078＞GOOD MANUFACTURING PRACTICES FOR BULK PHARMACEUTICAL EXCIPIENTS 批药品赋形剂的生产管理规范＜1079＞Good Storage and Shipping Practices 良好的贮存与运输规范＜1080＞BULK PHARMACEUTICAL EXCIPIENTS—CERTIFICATE OF ANALYSIS批药品赋形剂-COA＜1084＞GLYCOPROTEIN AND GLYCAN ANALYSIS—GENERAL CONSIDERATIONS 糖蛋白和多糖分析-一般通则＜1086＞IMPURITIES IN DRUG SUBSTANCES AND DRUG PRODUCTS药物和药物产品中的杂质＜1087＞APPARENT INTRINSIC DISSOLUTION—DISSOLUTION TESTING PROCEDURES FOR ROTATING DISK AND STATIONARY DISK内部的溶出度-旋转和静止溶出检测程序？＜1088＞IN VITRO AND IN VIVO EV ALUATION OF DOSAGE FORMS体内与体外的剂型的评估＜1090＞ASSESSMENT OF DRUG PRODUCT PERFORMANCE-BIOAV AILABILITY, BIOEQUIV ALENCE, AND DISSOLUTION药物产品性能评估：生物利用度、生物等效性和溶出＜1091＞LABELING OF INACTIVE INGREDIENTS非活性成分的标示＜1092＞THE DISSOLUTION PROCEDURE: DEVELOPMENT AND V ALIDATION溶出程序：开发与验证＜1094＞CAPSULES—DISSOLUTION TESTING AND RELATED QUALITY ATTRIBUTES 胶囊-关于产品质量的溶出测定＜1097＞BULK POWDER SAMPLING PROCEDURES：粉末样品取样程序＜1102＞IMMUNOLOGICAL TEST METHODS—GENERAL CONSIDERATIONS免疫测试方法-总则＜1103＞IMMUNOLOGICAL TEST METHODS—ENZYME-LINKED IMMUNOSORBENT ASSAY (ELISA) 免疫学测试方法-酶联免疫吸附测定＜1104＞IMMUNOLOGICAL TEST METHODS—IMMUNOBLOT ANALYSIS免疫测试方法-免疫印迹法＜1105＞IMMUNOLOGICAL TEST METHODS—SURFACE PLASMON RESONANCE 免疫测试方法-表面等离子体共振＜1106＞IMMUNOGENICITY ASSAYS—DESIGN AND VALIDATION OF IMMUNOASSAYS TO DETECT ANTI-DRUG ANTIBODIES？＜1111＞MICROBIOLOGICAL EXAMINATION OF NONSTERILE PRODUCTS: ACCEPTANCE CRITERIA FOR PHARMACEUTICAL PREPARATIONS AND SUBSTANCES FOR PHARMACEUTICAL USE非无菌产品的微生物学检查：药用制剂和制药过程使用的物质接受标准＜1112＞MICROBIAL CHARACTERIZATION, IDENTIFICATION, AND STRAIN TYPING 非无菌药物产品水活性测定应用＜1113＞MICROBIOLOGICAL ATTRIBUTES OF NONSTERILE PHARMACEUTICAL PRODUCTS 非无菌药品中的微生物分布＜1115＞BIOBURDEN CONTROL OF NONSTERILE DRUG SUBSTANCES AND PRODUCTS 非无菌药物和产品的生物负载控制＜1116＞MICROBIOLOGICAL CONTROL AND MONITORING OF ASEPTIC PROCESSING ENVIRONMENTS洁净的房间与其它可控环境的微生物评估＜1117＞MICROBIOLOGICAL BEST LABORATORY PRACTICES 微生物最优实验室规范＜1118＞MONITORING DEVICES—TIME, TEMPERATURE, AND HUMIDITY监控装置－时间、温度与湿度＜1119＞NEAR-INFRARED SPECTROPHOTOMETRY近红外分光光度测定法＜1120＞Raman Spectrophotometry 拉曼分光光度测定法＜1121＞NOMENCLATURE命名＜1125＞NUCLEIC ACID-BASED TECHNIQUES—GENERAL 核酸技术-通则＜1126＞NUCLEIC ACID-BASED TECHNIQUES—EXTRACTION, DETECTION, AND SEQUENCING 核酸技术-提取、检测、测序＜1127＞NUCLEIC ACID-BASED TECHNIQUES—AMPLIFICATION 核酸技术-扩增＜1128＞NUCLEIC ACID-BASED TECHNIQUES—MICROARRAY 核酸技术-微阵列＜1129＞NUCLEIC ACID-BASED TECHNIQUES—GENOTYPING 核酸技术-基因分型＜1130＞NUCLEIC ACID-BASED TECHNIQUES—APPROACHES FOR DETECTING TRACE NUCLEIC ACIDS (RESIDUAL DNA TESTING)核酸技术-探测微量核酸的应用（残留DNA测试）＜1136＞PACKAGING AND REPACKAGING—SINGLE-UNIT CONTAINERS包装和再包装－单一容器＜1151＞PHARMACEUTICAL DOSAGE FORMS药物剂型＜1152＞ANIMAL DRUGS FOR USE IN ANIMAL FEEDS兽药在动物饲料中的使用＜1160＞PHARMACEUTICAL CALCULATIONS IN PRESCRIPTION COMPOUNDING 按处方混合的药物的计算＜1163＞QUALITY ASSURANCE IN PHARMACEUTICAL COMPOUNDING按处方混合的药物的质量保证＜1171＞PHASE-SOLUBILITY ANALYSIS相溶解分析＜1174＞Powder Flow 粉末流动性＜1176＞PRESCRIPTION BALANCES AND VOLUMETRIC APPARATUS 处方天平与容量器具＜1177＞Good Packaging Practices 良好的包装操作＜1178＞Good Repackaging Practices 良好的再包装操作＜1180＞HUMAN PLASMA 人血浆＜1181＞SCANNING ELECTRON MICROSCOPY扫描电子显微镜＜1184＞SENSITIZATION TESTING 致敏测试＜1191＞STABILITY CONSIDERATIONS IN DISPENSING PRACTICE分装操作中稳定性考察＜1195＞SIGNIFICANT CHANGE GUIDE FOR BULK PHARMACEUTICAL EXCIPIENTS 散装药用辅料更换指导原则＜1197＞GOOD DISTRIBUTION PRACTICES FOR BULK PHARMACEUTICAL EXCIPIENTS 散装药用辅料良好的分装操作＜1207＞STERILE PRODUCT PACKAGING—INTEGRITY EV ALUATION无菌产品包装－完整性评估＜1208＞STERILITY TESTING—V ALIDATION OF ISOLATOR SYSTEMS无菌实验－隔离系统的验证＜1209＞STERILIZATION—CHEMICAL AND PHYSICOCHEMICAL INDICATORS AND INTEGRATORS灭菌－化学与物理化学的指示剂以及二者的综合＜1211＞STERILIZATION AND STERILITY ASSURANCE OF COMPENDIAL ARTICLES 药典物品中的灭菌与灭菌保证＜1216＞TABLET FRIABILITY片剂的脆碎度＜1217＞TABLET BREAKING FORCE 片剂断裂力＜1222＞TERMINALLY STERILIZED PHARMACEUTICAL PRODUCTS—PARAMETRIC RELEASE 药品终端灭菌－放行参数＜1223＞V ALIDATION OF ALTERNATIVE MICROBIOLOGICAL METHODS可供选择的微生物学方法的验证＜1224＞TRANSFER OF ANALYTICAL PROCEDURES 分析方法转移＜1225＞V ALIDATION OF COMPENDIAL PROCEDURES药典方法的验证＜1226＞VERIFICATION OF COMPENDIAL PROCEDURES 药典方法的确认＜1227＞V ALIDATION OF MICROBIAL RECOVERY FROM PHARMACOPEIAL ARTICLES从药物中回收微生物的验证＜1229＞STERILIZATION OF COMPENDIAL ARTICLES 药典灭菌过程＜1229.1＞STEAM STERILIZATION BY DIRECT CONTACT 直接蒸汽灭菌＜1229.2＞MOIST HEAT STERILIZATION OF AQUEOUS LIQUIDS 水溶液的湿热灭菌＜1229.3＞MONITORING OF BIOBURDEN 生物负载监控＜1229.4＞STERILIZING FILTRATION OF LIQUIDS 溶液的无菌过滤器＜1229.6＞LIQUID-PHASE STERILIZATION 液态灭菌＜1229.7＞GASEOUS STERILIZATION 气态灭菌＜1229.8＞DRY HEAT STERILIZATION 干热灭菌＜1229.10＞RADIATION STERILIZATION 辐射灭菌＜1230＞W ATER FOR HEMODIALYSIS APPLICATIONS 血液透析过程用水＜1231＞W ATER FOR PHARMACEUTICAL PURPOSES制药用水＜1234＞VACCINES FOR HUMAN USE—POLYSACCHARIDE AND GLYCOCONJUGATE VACCINES 人用疫苗-多糖和糖复合物疫苗＜1235＞V ACCINES FOR HUMAN USE—GENERAL CONSIDERATIONS 人用疫苗-通则＜1237＞VIROLOGY TEST METHODS 病毒测试方法＜1238＞V ACCINES FOR HUMAN USE—BACTERIAL V ACCINES 人用疫苗-细菌疫苗＜1240＞VIRUS TESTING OF HUMAN PLASMA FOR FURTHER MANUFACTURE下一步使用人血浆的病毒测试＜1241＞W ATER–SOLID INTERACTIONS IN PHARMACEUTICAL SYSTEMS在药物系统中水与固体的相互作用＜1251＞WEIGHING ON AN ANALYTICAL BALANCE关于分析天平的称重＜1265＞Written Prescription Drug Information－Guidelines 书面的处方药信息－指南＜1285＞PREPARATION OF BIOLOGICAL SPECIMENS FOR HISTOLOGIC AND IMMUNOHISTOCHEMICAL ANALYSIS为了组织和免疫组织分析的生物标本制备＜1285.1＞HEMATOXYLIN AND EOSIN STAINING OF SECTIONED TISSUE FOR MICROSCOPIC EXAMINATION显微镜观察用苏木精和伊红染色的切片＜1601＞PRODUCTS FOR NEBULIZATION—CHARACTERIZATION TESTS 产品雾化状态-性状描述＜1644＞THEORY AND PRACTICE OF ELECTRICAL CONDUCTIVITY MEASUREMENTS OF SOLUTIONS溶液电导值测量方法的理论与实践＜1660＞EV ALUATION OF THE INNER SURFACE DURABILITY OF GLASS CONTAINERS 玻璃容器内表面耐久性评估＜1724＞SEMISOLID DRUG PRODUCTS—PERFORMANCE TESTS 半固态药物产品-性能测试＜1736＞APPLICATIONS OF MASS SPECTROMETRY 质谱应用＜1761＞APPLICATIONS OF NUCLEAR MAGNETIC RESONANCE SPECTROSCOPY核磁共振光谱应用＜1787＞MEASUREMENT OF SUBVISIBLE PARTICULATE MATTER IN THERAPEUTIC PROTEIN INJECTIONS用显微镜测量方法测量治疗性蛋白注射剂的不溶性微粒＜1788＞METHODS FOR THE DETERMINATION OF PARTICULATE MATTER IN INJECTIONS AND OPHTHALMIC SOLUTIONS注射剂和眼用溶液的不溶性微粒测定的方法选择＜1852＞ATOMIC ABSORPTION SPECTROSCOPY—THEORY AND PRACTICE原子吸收光谱-理论与实践＜1853＞FLUORESCENCE SPECTROSCOPY—THEORY AND PRACTICE荧光光谱-理论与实践＜1854＞MID-INFRARED SPECTROSCOPY—THEORY AND PRACTICE中红外光谱-理论与实践＜1857＞ULTRA VIOLET-VISIBLE SPECTROSCOPY—THEORY AND PRACTICE紫外可见光谱-理论与实践＜1911＞RHEOMETRY 流变测定Dietary Supplements营养补充剂General Tests and Assays 一般检查法与测定法＜2021＞MICROBIAL ENUMERATION TESTS—NUTRITIONAL AND DIETARY SUPPLEMENTS…3080微生物数量实验－营养与食品添加剂＜2022＞MICROBIOLOGICAL PROCEDURES FOR ABSENCE OF SPECIFIED MICROORGANISMS—NUTRITIONAL AND DIETARY SUPPLEMENTS (3083)不得检出特定微生物的程序－营养与营养补充剂＜2023>MICROBIOLOGICAL ATTRIBUTES OF NONSTERILE NUTRITIONAL AND DIETARY SUPPLEMENTS……3087非无菌的营养与食品添加剂中的微生物分布<2040>DISINTEGRATION AND DISSOLUTION OF DIETARY SUPPLEMENTS (3089)食品添加剂的崩解与溶出<2091>WEIGHT V ARIATION OF DIETARY SUPPLEMENTS……3092食品添加剂的重量差异<2750>MANUFACTURING PRACTICES FOR DIETARY SUPPLEMENTS (3093)食品添加剂的生产操作。

VALIDATION OF COMPENDIAL PROCEDURES 药典方法的验证Test procedures for assessment of the quality levels of pharmaceutical articles are subject to various requirements. According to Section 501 of the Federal Food, Drug, and Cosmetic Act, assays and specifications in monographs of the United States Pharmacopeia and the National Formulary constitute legal standards. The Current Good Manufacturing Practice regulations [21 CFR 211.194(a)] require that test methods, which are used for assessing compliance of pharmaceutical articles with established specifications, must meet proper standards of accuracy and reliability. Also, according to these regulations [21 CFR 211.194(a)(2)], users of analytical methods describedin USP–NF are not required to validate the accuracy and reliability of these methods, but merely verify their suitability under actual conditions of use. Recognizing the legal status of USP and NF standards, it is essential, therefore, that proposals for adoption of new or revised compendial analytical procedures be supported by sufficient laboratory data to document their validity.用于评估药品质量的检验方法需要满足不同的要求。

《 671》包装容器——性能检测本章规定了用来包装的塑料容器及其组件功能性质上的标准(药品、生物制剂、营养补充剂和医疗器械 )，定义了保存、包装、存储和标签方面的凡例与要求。

本文提供的试验用于确定塑料容器的透湿性和透光率。

盛装胶囊和片剂的多单元容器章节适用于多单元容器。

盛装胶囊和片剂的单位剂量容器章节适用于单位剂量容器。

盛装胶囊和片剂的多单元容器 (没有密封 ) 的章节适用于没有密封的聚乙烯和聚丙烯容器。

盛装液体的多元和单元容器的章节适用于多元的和单元的容器。

一个容器想要提供避光保护或作为一个符合耐光要求的容器，由具有耐光的特殊性质的材料组成，包括任何涂层应用。

一个无色透明或半透明的容器通过一个不透明的外壳包装变成耐光的 (见凡例和要求 )，可免于对光的透射要求。

在多单元容器和封盖与水泡的单位剂量容器由衬垫密封情况下，此处使用的术语“容器”指的是整个系统的组成。

盛装胶囊和片剂的多元容器干燥剂——放置一些颗粒 4— 8 目的无水氯化钙在一个浅的容器里，仔细剔除细粉，然后置于110°干燥，并放在干燥器中冷却。

试验过程——挑选 12 个类型和尺寸一致的容器，用不起毛的毛巾清洁密闭表面，并打开和关闭每个容器 30 次。

坚决每次应用容器密闭一致。

通过扭矩关闭螺旋盖容器，使气密性在附表规定的范围内。

10 个指定的测试容器添加干燥剂，如果容器容积大于等于20mL，每个填充 13mm以内封闭；如果容器的容积小于 20 毫升，每个填充容器容量的三分之二。

如果容器内部的深度超过 63mm，惰性填料或垫片可以放置在底部来最小化容器和干燥剂的总重量；干燥剂层在这样一个容器中深度不低于 5cm。

添加干燥剂之后，立即按附表中规定的扭矩封闭螺旋帽容器。

剩余的 2 个指定为对照容器，每个添加足够数量的玻璃珠，重量约等于每个测试容器的重量，并用附表中规定的扭矩封闭螺旋帽容器。

记录各个容器的重量，如果容器的容积小于 20 毫升，精确到 0.1 毫克；如果容器容积为 20 毫升或以上但小于 200 毫升，精确到毫克；如果容器容积为 200 毫升及以上，精确到厘克（10 毫克）；在相对湿度 75±3%和温度 23±2°的环境下存储。

USP微生物限度检查中文USP微生物限度检查中文61）微生物限度检测（MICROBIAL LIMIT TESTS）此章提供方法来检测可能存在的好氧微生物其他制药过程中可能出现的微生物的数量，包括原材料和成品中的。

如果经过验证确认可以得到相同或更好的检测结论，也允许采用自动化的检测方法。

在样品检测过程中须进行无菌操作。

若无特别说明，则“培养（incubate）”一词指在30—35℃的培养箱内培养24至48小时；“生长（growth）”一词用于专门的判定，说明“存在和可能存在活的微生物”。

准备实验 (Preparatory Testing)本章涉及实验结果的有效性取决于：提供的被检测样品本身在实验条件下，被充分证明不会抑制可能存在的微生物的生长。

因此，在准备样品时，需要正规的实验操作和符合要求的实验条件，接种稀释样品到含有以下（微生物）培养物的培养基：金黄色（奥里斯）葡萄球菌（Staphylococcus aureus）,大肠埃希氏菌（Escherichia coli）, 铜绿假单胞菌(Pseudomonas aeruginosa), 和沙门氏菌（Salmonella）。

方法如下：将用肉汤培养基培养24小时后的（微生物）不小于10-3稀释的微生物培养物，加1 ml（微生物）培养液到磷酸(盐)缓冲液(pH 7.2)，液体大豆酪蛋白消化物培养基（Fluid Soybean-Casein Digest Medium），或者液体乳糖培养基（Fluid Lactose Medium）。

相应培养基培养失败则需要采取以下方法更改检测程序：（1）增加稀释液体积，检测样品加入量仍维持不变；或者（2）中和一定数量的干扰因子；或者（3）结合（1）、（2）得出适当条件，使接种物得以生长。

以下是一些物质的成分和浓度，该物质及浓度可用于加入培养基、阻止物质发挥抑菌作用：大豆卵磷脂（soy lecithin, 0.5%）或者聚山梨醇酯20（polysorbate 20, 4.0%）。

《671》包装容器——性能检测本章规定了用来包装的塑料容器及其组件功能性质上的标准(药品、生物制剂、营养补充剂和医疗器械)，定义了保存、包装、存储和标签方面的凡例与要求。

本文提供的试验用于确定塑料容器的透湿性和透光率。

盛装胶囊和片剂的多单元容器章节适用于多单元容器。

盛装胶囊和片剂的单位剂量容器章节适用于单位剂量容器。

盛装胶囊和片剂的多单元容器(没有密封) 的章节适用于没有密封的聚乙烯和聚丙烯容器。

盛装液体的多元和单元容器的章节适用于多元的和单元的容器。

一个容器想要提供避光保护或作为一个符合耐光要求的容器，由具有耐光的特殊性质的材料组成，包括任何涂层应用。

一个无色透明或半透明的容器通过一个不透明的外壳包装变成耐光的(见凡例和要求 )，可免于对光的透射要求。

在多单元容器和封盖与水泡的单位剂量容器由衬垫密封情况下，此处使用的术语“容器”指的是整个系统的组成。

盛装胶囊和片剂的多元容器干燥剂——放置一些颗粒4—8目的无水氯化钙在一个浅的容器里，仔细剔除细粉，然后置于110°干燥，并放在干燥器中冷却。

试验过程——挑选12个类型和尺寸一致的容器，用不起毛的毛巾清洁密闭表面，并打开和关闭每个容器30次。

坚决每次应用容器密闭一致。

通过扭矩关闭螺旋盖容器，使气密性在附表规定的范围内。

10个指定的测试容器添加干燥剂，如果容器容积大于等于20mL，每个填充13mm以内封闭；如果容器的容积小于20毫升，每个填充容器容量的三分之二。

如果容器内部的深度超过63mm，惰性填料或垫片可以放置在底部来最小化容器和干燥剂的总重量；干燥剂层在这样一个容器中深度不低于5cm。

添加干燥剂之后，立即按附表中规定的扭矩封闭螺旋帽容器。

剩余的2个指定为对照容器，每个添加足够数量的玻璃珠，重量约等于每个测试容器的重量，并用附表中规定的扭矩封闭螺旋帽容器。

记录各个容器的重量，如果容器的容积小于20毫升，精确到0.1毫克；如果容器容积为20毫升或以上但小于200毫升，精确到毫克；如果容器容积为200毫升及以上，精确到厘克（10毫克）；在相对湿度75±3%和温度23±2°的环境下存储。

美国药典－中英文对照译文美国药典中记载的辣椒碱资料辣椒碱（辣椒素）分子结构式：C18H27NO3，分子量：305.41，化学名：（反）－N－[（4－N－羟基－3－甲氧基苯基）－甲基]－8－甲基－6－壬烯基酰胺以干燥提取物计算，辣椒碱含辣椒二萜类化合物总量为标示量的90％－100%,其中辣椒素的含量达到50％以上，辣椒素和二氢辣椒素总量超过75％，其它辣椒素类化合物总量不足15％。

注意事项：小心处置辣椒碱，谨防吸入辣椒碱微粒，勿使身体接触辣椒碱。

包装贮藏：密封包装，置避光，阴凉处保存。

标示量：以辣椒二萜类化合物总百分含量表示。

美国药典参考标准：美国药典辣椒素标准规范，美国药典二氢辣椒素标准规范。

鉴别：配制1.0mg/ml辣椒碱甲醇溶液，配制符合美国药典标准的辣椒碱1.0mg/ml甲醇溶液作为对照液，分别点样于0.25mm厚硅胶、凝胶混合薄层板上，点样量为10礚，将薄层板放于乙醚－甲醇（19:1）展开剂中展开，待展开剂前沿至薄层板3/4处时将薄层板取出，晾干，用0.5% 2,6-二溴苯醌-氯化亚胺甲醇溶液喷雾显色，放于氨气中片刻，取出，鉴别色谱图：供试液主要斑点颜色（兰色）及R值与对照液主要斑点颜色（兰色）及R值一致。

熔点〈741〉: 57°－66°, 一般熔融起始温度至结束温度温差不超过5°。

干燥失重〈731〉: 置40°P2O5真空干燥器中干燥5小时，失重不超过1.0%。

灼烧残渣：≤1.0％。

辣椒素，二氢辣椒素及其它辣椒二萜类化合物含量测定：流动相：磷酸水溶液（l ：1000，V/V）：乙腈(600:400)混匀，0.5祄微孔滤膜滤过，脱气。

流动相视色谱行为可作适当调整。

辣椒素对照液：精密称取美国药典标准的辣椒碱适量溶于甲醇中，配制约0.1 mg/mL的辣椒甲醇溶液。

二氢辣椒素对照液：精密称取美国药典标准的辣椒碱适量溶于甲醇中，配制约0.025mg/mL的辣椒甲醇溶液。

921WATERDETERMINATION水分测定Many Pharmacopeial articles either are hydrates or contain water in adsorbed form. As a result, the determination of the water content is important in demonstrating compliance with the Pharmacopeial standards. Generally one of the methods given below is called for in the individual monograph, depending upon the nature of the article. In rare cases, a choice is allowed between two methods. When the article contains water of hydration, the Method I (Titrimetric), the Method II (Azeotropic), or the Method III (Gravimetric) is employed, as directed in the individual monograph, and the requirement is given under the heading Water.很多药典物品要么是水合物，要么含有处于吸附状态的水。

因此，测定水分含量对于证实与药典标准的符合性是很重要的。

通常，在具体的各论中会根据该物品的性质，要求使用下面若干方法中的一个。

偶尔，会允许在2个方法中任选一个。

当该物品含有水合状态的水，按照具体各论中的规定，使用方法I（滴定测量法）、方法II（恒沸测量法）、或方法III（重量分析法），这个要求在标题水分项下给出。

USP36 1117 优良微生物检测规范（中英文1/ 2）2013-08-09 15:30:46| 分类：USP|举报|字号订阅1117 MICROBIOLOGICAL BEST LABORATORY PRACTICES 优良微生物检测规范INTRODUCTION 介绍Good laboratory practices in a microbiology laboratory consist of activities that depend on several principles: aseptic technique, control of media, control of test strains, operation and control of equipment, diligent recording and evaluation of data, and training of the laboratory staff. Because of the inherent risk of variability in microbiology data, reliability and reproducibility are dependent on the use of accepted methods and adherence to good laboratory practices.优良微生物检测规范由一些活动组成，这些活动依赖于几个基本要素：无菌技术、培养基控制、检测用菌株控制、设备操作和控制、完善的记录和数据评估、化验室员工的培训。

由于微生物数据具有天生的不确定性，数据的可靠性和重复性取决于是否使用被接受的方法，以及是否严格遵守化验室规范。

MEDIA PREPARATION AND QUALITY CONTROL 培养基制备和质量控制Media Preparation 培养基制备Culture media are the basis for most microbiological tests. Safeguarding the quality of the media is therefore critical to the success of the microbiology laboratory. Media preparation, proper storage, and quality control testing can ensure a consistent supply of high-quality media.培养基是大多数微生物测试的基础。

661 CONTAINERS—PLASTICSINTRODUCTIONIt is the purpose of this chapter to provide standards for plastic materials and components used to package medical articles (pharmaceuticals, biologics, dietary supplements, and devices). Definitions that apply to this chapter are provided in the Preservation, Packaging, Storage, and Labeling section of the General Notices and Requirements. Standards and tests for the functional properties of containers and their components areprovided in general chapter Containers—Performance Testing 671.In addition to the standards provided herein, the ingredients added to the polymers, and those used in the fabrication of the containers, must conform to the requirements in the applicable sections of the Code of Federal Regulations, Title 21, Indirect Food Additives, or have been evaluated by the FDA and determined to be acceptable substances for the listed use.Plastic articles are identified and characterized by IR spectroscopy and differential scanning calorimetry. Standards are provided in this chapter for the identification and characterization of the different types of plastic, and the test procedures are provided at the end of the chapter. The degree of testing is based on whether or not the container has direct contact with the drug product, and the risk is based on the route of administration.Plastics are composed of a mixture of homologous polymers, having a range of molecular weights. Plastics may contain other substances such as residues from the polymerization process, plasticizers, stabilizers, antioxidants, pigments, and lubricants. These materials meet the requirements for food contact as provided in the Code of Federal Regulations, Title 21. Factors such as plastic composition, processing and cleaning procedures, surface treatment, contacting media, inks, adhesives, absorption and permeability of preservatives, and conditions of storage may also affect the suitability of a plastic for a specific use. Extraction tests are designed to characterize the extracted components and identify possible migrants. The degree or extent of testing for extractables of the component is dependent on the intended use and the degree of risk to adversely impact the efficacy of the compendial article (drug, biologic, dietary supplement, or device). Resin-specific extraction tests are provided in this chapter for polyethylene, polypropylene, polyethylene terephthalate, and polyethylene terephthalate G. Test all other plastics as directed for Physicochemical Tests in the section Test Methods. Conduct the Buffering Capacity test only when the containers are intended to hold a liquid product.Plastic components used for products of high risk, such as those intended for inhalation, parenteral preparation, and ophthalmics are tested using the Biological Tests in thesection Test Methods.Plastic containers intended for packaging products prepared for parenteral use meet the requirements for Biological Tests and Physicochemical Tests in the section Test Methods. Standards are also provided for polyethylene containers used to package dry oral dosage forms that are not meant for constitution into solution.POLYETHYLENE CONTAINERSScopeThe standards and tests provided in this section characterize containers and components, produced from either low-density polyethylene or high-density polyethylene of either homopolymer or copolymer resins that are interchangeably suitable for packaging dry oral dosage forms not meant for constitution into solution. All polyethylene components are subject to testing by IR spectroscopy and differential scanning calorimetry. Where stability studies have been performed to establish the expiration date of a particular dosage form in the appropriate polyethylene container, then any other polyethylene container meeting these requirements may be similarly used to package such a dosage form, provided that the appropriate stability programs are expanded to include the alternative container, in order to ensure that the identity, strength, quality, and purity of the dosage form are maintained throughout the expiration period.BackgroundHigh-density and low-density polyethylene are long-chain polymers synthesized under controlled conditions of heat and pressure, with the aid of catalysts from not less than 85.0% ethylene and not less than 95.0% total olefins. Other olefin ingredients that are most frequently used are butene, hexene, and propylene. High-density polyethylene and low-density polyethylene both have an IR absorption spectrum that is distinctive for polyethylene, and each possesses characteristic thermal properties. High-density polyethylene has a density between 0.941 and 0.965 g per cm3. Low-density polyethylene has a density between 0.850 and 0.940 g per cm3. Other properties that may affect the suitability of polyethylene include modulus of elasticity, melt index, environmental stress crack resistance, and degree of crystallinity after molding.High-Density PolyethyleneInfrared Spectroscopy— Proceed as directed for Multiple Internal Reflectance in the section Test Methods. The corrected spectrum of the specimen exhibits major absorption bands only at the same wavelengths as the spectrum of USP High-Density Polyethylene RS.Differential Scanning Calorimetry— Proceed as directed for Thermal Analysis in the section Test Methods. The thermogram of the specimen is similar to the thermogram ofUSP High-Density Polyethylene RS, similarly determined, and the temperature of the endotherm (melt) in the thermogram of the specimen does not differ from that of the USP Reference Standard by more than 6.0.Heavy Metals and Nonvolatile Residue— Prepare extracts of specimens for these tests as directed for Physicochemical Tests under Test Methods, except that for each 20.0 mL of Extracting Medium the portion shall be 60 cm2, regardless of thickness.HEAVY METALS— Containers meet the requirements for Heavy Metals in the section Physicochemical Tests under Test Methods.NONVOLATILE RESIDUE— Proceed as directed for Nonvolatile Residue under Physicochemical Tests, except that the Blank shall be the same solvent used in each of the following test conditions: the difference between the amounts obtained from the Sample Preparation and the Blank does not exceed 12.0 mg when water maintained at a temperature of 70 is used as the Extracting Medium; does not exceed 75.0 mg when alcohol maintained at a temperature of 70 is used as the Extracting Medium; and does not exceed 100.0 mg when hexanes maintained at a temperature of 50 is used as the Extracting Medium.Components Used in Contact with Oral Liquids— Proceed as directed for Buffering Capacity in the section Physicochemical Tests under Test Methods.Low-Density PolyethyleneInfrared Spectroscopy— Proceed as directed for Multiple Internal Reflectance under Test Methods. The corrected spectrum of the specimen exhibits major absorption bands only at the same wavelengths as the spectrum of USP Low-Density Polyethylene RS.Differential Scanning Calorimetry— Proceed as directed for Thermal Analysis under Test Methods. The thermogram of the specimen is similar to the thermogram of USP Low-Density Polyethylene RS, similarly determined, and the temperature of the endotherm (melt) in the thermogram of the specimen does not differ from that of the USP Reference Standard by more than 8.0.Heavy Metals and Nonvolatile Residue— Prepare extracts of specimens for these tests as directed for Sample Preparation in the section Physicochemical Tests under Test Methods, except that for each 20.0 mL of Extracting Medium the portion shall be 60 cm2, regardless of thickness.HEAVY METALS— Containers meet the requirements for Heavy Metals in the section Physicochemical Tests under Test Methods.NONVOLATILE RESIDUE— Proceed as directed for Nonvolatile Residue in the section Physicochemical Tests under Test Methods, except that the Blank shall be the same solvent used in each of the following test conditions: the difference between the amountsobtained from the Sample Preparation and the Blank does not exceed 12.0 mg when water maintained at a temperature of 70 is used as the Extracting Medium; does not exceed 75.0 mg when alcohol maintained at a temperature of 70 is used as the Extracting Medium; and does not exceed 350.0 mg when hexanes maintained at a temperature of 50 is used as the Extracting Medium.Components Used in Contact with Oral Liquids— Proceed as directed for Buffering Capacity in the section Physicochemical Tests under Test Methods.POLYPROPYLENE CONTAINERSScopeThe standards and tests provided in this section characterize polypropylene containers, produced from either homopolymers or copolymers, that are interchangeably suitable for packaging dry solid and liquid oral dosage forms. Where suitable stability studies have been performed to establish the expiration date of a particular dosage form in the appropriate polypropylene container, then any other polypropylene container meeting these requirements may be similarly used to package such a dosage form, provided that the appropriate stability programs are expanded to include the alternative container, in order to ensure that the identity, strength, quality, and purity of the dosage form are maintained throughout the expiration period.BackgroundPropylene polymers are long-chain polymers synthesized from propylene or propylene and other olefins under controlled conditions of heat and pressure, with the aid of catalysts. Examples of other olefins most commonly used include ethylene and butene. The propylene polymers, the ingredients used to manufacture the propylene polymers, and the ingredients used in the fabrication of the containers conform to the applicable sections of the Code of Federal Regulations, Title 21.Factors such as plastic composition, processing and cleaning procedures, contacting media, inks, adhesives, absorption, adsorption and permeability of preservatives, and conditions of storage may also affect the suitability of a plastic for a specific use. The suitability of a specific polypropylene must be established by appropriate testing. Polypropylene has a distinctive IR spectrum and possesses characteristic thermal properties. It has a density between 0.880 and 0.913 g per cm3. The permeation properties of molded polypropylene containers may be altered when reground polymer is incorporated, depending on the proportion of reground material in the final product. Other properties that may affect the suitability of polypropylene used in containers for packaging drugs are the following: oxygen and moisture permeability, modulus of elasticity, melt flow index, environmental stress crack resistance, and degree ofcrystallinity after molding. The requirements in this section are to be met when dry solid and liquid oral dosage forms are to be packaged in a container defined by this section.Infrared Spectroscopy— Proceed as directed for Multiple Internal Reflectance under Test Methods. The corrected spectrum of the specimen exhibits major absorption bands only at the same wavelengths as the spectrum of the respective USP Homopolymer Polypropylene RS or copolymer polypropylene standard, similarly determined.Differential Scanning Calorimetry— Proceed as directed for Thermal Analysis under Test Methods. The temperature of the endotherm (melt) in the thermogram does not differ from that of the USP Reference Standard for homopolymers by more than 6.0. The temperature of the endotherm obtained from the thermogram of the copolymer polypropylene specimen does not differ from that of the copolymer polypropylene standard by more than 12.0.Heavy Metals and Nonvolatile Residue— Prepare extracts of specimens for these tests as directed for Sample Preparation in the section Physicochemical Tests under Test Methods, except that for each 20 mL of Extracting Medium the portion shall be 60 cm2, regardless of thickness.HEAVY METALS— Containers meet the requirements for Heavy Metals in the section Physicochemical Tests under Test Methods.NONVOLATILE RESIDUE— Proceed as directed for Nonvolatile Residue in the section Physicochemical Tests under Test Methods, except that the Blank shall be the same solvent used in each of the following test conditions: the difference between the amounts obtained from the Sample Preparation and the Blank does not exceed 10.0 mg when water maintained at a temperature of 70 is used as the Extracting Medium; does not exceed 60.0 mg when alcohol maintained at a temperature of 70 is used as the Extracting Medium; and does not exceed 225.0 mg when hexanes maintained at a temperature of 50 is used as the Extracting Medium. Containers meet these requirements for Nonvolatile Residue for all of the above extracting media. [N OTE—Hexanes and alcohol are flammable. When evaporating these solvents, use a current of air with the water bath; when drying the residue, use an explosion-proof oven. ]Components Used in Contact with Oral Liquids— Proceed as directed for Buffering Capacity in the section Physicochemical Tests under Test Methods.POLYETHYLENE TEREPHTHALATE BOTTLES AND POLYETHYLENETEREPHTHALATE G CONTAINERSScopeThe standards and tests provided in this section characterize polyethylene terephthalate(PET) and polyethylene terephthalate G (PETG) bottles that are interchangeably suitable for packaging liquid oral dosage forms. Where stability studies have been performed to establish the expiration date of a particular liquid oral dosage form in a bottle meeting the requirements set forth herein for either PET or PETG bottles, any other PET or PETG bottle meeting these requirements may be similarly used to package such a dosage form, provided that the appropriate stability programs are expanded to include the alternative bottle in order to ensure that the identity, strength, quality, and purity of the dosage form are maintained throughout the expiration period. The suitability of a specific PET or PETG bottle for use in the dispensing of a particular pharmaceutical liquid oral dosage form must be established by appropriate testing.BackgroundPET resins are long-chain crystalline polymers prepared by the condensation of ethylene glycol with dimethyl terephthalate or terephthalic acid. PET copolymer resins are prepared in a similar way, except that they may also contain a small amount of either isophthalic acid (not more than 3 mole percent) or 1,4-cyclohexanedimethanol (not more than 5 mole percent). Polymerization is conducted under controlled conditions of heat and vacuum, with the aid of catalysts and stabilizers.PET copolymer resins have physical and spectral properties similar to PET and for practical purposes are treated as PET. The tests and specifications provided in this section to characterize PET resins and bottles apply also to PET copolymer resins and to bottles fabricated from them.PET and PET copolymer resins generally exhibit a large degree of order in their molecular structure. As a result, they exhibit characteristic composition-dependent thermal behavior, including a glass transition temperature of about 76 and a melting temperature of about 250. These resins have a distinctive IR absorption spectrum that allows them to be distinguished from other plastic materials (e.g., polycarbonate, polystyrene, polyethylene, and PETG resins). PET and PET copolymer resins have a density between 1.3 and 1.4 g per cm3and a minimum intrinsic viscosity of 0.7 dL per g, which corresponds to a number average molecular weight of about 23,000 Da.PETG resins are high molecular weight polymers prepared by the condensation of ethylene glycol with dimethyl terephthalate or terephthalic acid and 15 to 34 mole percent of 1,4-cyclohexanedimethanol. PETG resins are clear, amorphous polymers, having a glass transition temperature of about 81 and no crystalline melting point, as determined by differential scanning calorimetry. PETG resins have a distinctive IR absorption spectrum that allows them to be distinguished from other plastic materials, including PET. PETG resins have a density of approximately 1.27 g per cm3 and a minimum intrinsic viscosity of 0.65 dL per g, which corresponds to a number average molecular weight of about 16,000 Da.PET and PETG resins, and other ingredients used in the fabrication of these bottles,conform to the requirements in the applicable sections of the Code of Federal Regulations, Title 21, regarding use in contact with food and alcoholic beverages. PET and PETG resins do not contain any plasticizers, processing aids, or antioxidants. Colorants, if used in the manufacture of PET and PETG bottles, do not migrate into the contained liquid.Infrared Spectroscopy— Proceed as directed under Multiple Internal Reflectance in the section Test Methods. The corrected spectrum of the specimen exhibits major absorption bands only at the same wavelengths as the spectrum of USP Polyethylene Terephthalate RS, or USP Polyethylene Terephthalate G RS, similarly determined.Differential Scanning Calorimetry— Proceed as directed under Thermal Analysis in the section Test Methods. For polyethylene terephthalate, the thermogram of the specimen is similar to the thermogram of USP Polyethylene Terephthalate RS, similarly determined: the melting point (T) of the specimen does not differ from that of the USP Referencem) of the specimen Standard by more than 9.0, and the glass transition temperature (Tgdoes not differ from that of the USP Reference Standard by more than 4.0. For polyethylene terephthalate G, the thermogram of the specimen is similar to the thermogram of USP Polyethylene Terephthalate G RS, similarly determined: the glass transition temperature (T) of the specimen does not differ from that of the USPgReference Standard by more than 6.0.Colorant Extraction— Select three test bottles. Cut a relatively flat portion from the side wall of one bottle, and trim it as necessary to fit the sample holder of the spectrophotometer. Obtain the visible spectrum of the side wall by scanning the portion of the visible spectrum from 350 to 700 nm. Determine, to the nearest 2 nm, the wavelength of maximum absorbance. Fill the remaining two test bottles, using 50% alcohol for PET bottles and 25% alcohol for PETG bottles. Fit the bottles with impervious seals, such as aluminum foil, and apply closures. Fill a glass bottle having the same capacity as that of the test bottles with the corresponding solvent, fit the bottle with an impervious seal, suchas aluminum foil, and apply a closure. Incubate the test bottles and the glass bottle at 49 for 10 days. Remove the bottles, and allow them to equilibrate to room temperature. Concomitantly determine the absorbances of the test solutions in 5-cm cells at the wavelength of maximum absorbance (see Spectrophotometry and Light–Scattering 851 ), using the corresponding solvent from the glass bottle as the blank. The absorbance values so obtained are less than 0.01 for both test solutions.Heavy Metals, Total Terephthaloyl Moieties, and Ethylene Glycol—EXTRACTING MEDIA—Purified Water— (see monograph).50 Percent Alcohol— Dilute 125 mL of alcohol with water to 238 mL, and mix.25 Percent Alcohol— Dilute 125 mL of 50 Percent Alcohol with water to 250 mL, and mix.n-Heptane.GENERAL PROCEDURE— [N OTE—Use an Extracting Medium of 50 Percent Alcohol for PET bottles and 25 Percent Alcohol for PETG bottles. ] For each Extracting Medium, fill a sufficient number of test bottles to 90% of their nominal capacity to obtain not less than 30 mL. Fill a corresponding number of glass bottles with Purified Water, a corresponding number of glass bottles with 50 Percent Alcohol or 25 Percent Alcohol, and a corresponding number of glass bottles with n-Heptane for use as Extracting Media blanks. Fit the bottles with impervious seals, such as aluminum foil, and apply closures. Incubate the test bottles and the glass bottles at 49 for 10 days. Remove the test bottles with the Extracting Media samples and the glass bottles with the Extracting Media blanks, and store them at room temperature. Do not transfer the Extracting Media samples to alternative storage vessels.HEAVY METALS— Pipet 20 mL of the Purified Water extract of the test bottles, filtered if necessary, into one of two matched 50-mL color-comparison tubes, and retain the remaining Purified Water extract in the test bottles for use in the test for Ethylene Glycol. Adjust the extract with 1 N acetic acid or 6 N ammonium hydroxide to a pH between 3.0 and 4.0, using short-range pH paper as an external indicator. Dilute with water to about 35 mL, and mix.Into the second color-comparison tube, pipet 2 mL of freshly prepared (on day of use)Standard Lead Solution (see Heavy Metals 231), and add 20 mL of Purified Water. Adjust with 1 N acetic acid or 6 N ammonium hydroxide to a pH between 3.0 and 4.0, using short-range pH paper as an external indicator. Dilute with water to about 35 mL, and mix.To each tube add 1.2 mL of thioacetamide–glycerin base TS and 2 mL of pH 3.5 AcetateBuffer (see Heavy Metals 231), dilute with water to 50 mL, and mix: any color produced within 10 minutes in the tube containing the Purified Water extract of the test bottles does not exceed that in the tube containing the Standard Lead Solution, both tubes being viewed downward over a white surface (1 ppm in extract).TOTAL TEREPHTHALOYL MOIETIES— Determine the absorbance of the 50 Percent Alcohol or 25 Percent Alcohol extract in a 1-cm cell at the wavelength of maximum absorbance atabout 244 nm (see Spectrophotometry and Light–Scattering 851), using as the blank the corresponding Extracting Medium blank: the absorbance of the extract does not exceed 0.150, corresponding to not more than 1 ppm of total terephthaloyl moieties. Determine the absorbance of the n-Heptane extract in a 1-cm cell at the wavelength of maximum absorbance at about 240 nm (see Spectrophotometry and Light-Scattering 851), using as the blank the n-Heptane Extracting Medium: the absorbance of theextract does not exceed 0.150, corresponding to not more than 1 ppm of total terephthaloyl moieties.ETHYLENE GLYCOL—Periodic Acid Solution— Dissolve 125 mg of periodic acid in 10 mL of water.Dilute Sulfuric Acid— To 50 mL of water add slowly and with constant stirring 50 mL of sulfuric acid, and allow to cool to room temperature.Sodium Bisulfite Solution— Dissolve 0.1 g of sodium bisulfite in 10 mL of water. Use this solution within 7 days.Disodium Chromotropate Solution— Dissolve 100 mg of disodium chromotropate in 100 mL of sulfuric acid. Protect this solution from light, and use within 7 days.Standard Solution— Dissolve an accurately weighed quantity of ethylene glycol in water, and dilute quantitatively, and stepwise if necessary, to obtain a solution having a known concentration of about 1 µg per mL.Test Solution— Use the Purified Water extract.Procedure— Transfer 1.0 mL of the Standard Solution to a 10-mL volumetric flask. Transfer 1.0 mL of the Test Solution to a second 10-mL volumetric flask. Transfer 1.0 mL of the Purified Water Extracting Medium to a third 10-mL volumetric flask. To each of the three flasks, add 100 µL of Periodic Acid Solution, swirl to mix, and allow to stand for 60 minutes. Add 1.0 mL of Sodium Bisulfite Solution to each flask, and mix. Add 100 µL of Disodium Chromotropate Solution to each flask, and mix. [N OTE—All solutions should be analyzed within 1 hour after addition of the Disodium Chromotropate Solution. ] Cautiously add 6 mL of sulfuric acid to each flask, mix, and allow the solutions to cool to room temperature. [Caution–Dilution of sulfuric acid produces substantial heat and can cause the solution to boil. Perform this addition carefully. Sulfur dioxide gas will be evolved. Use of a fume hood is recommended.] Dilute each solution with Dilute Sulfuric Acid to volume, and mix. Concomitantly determine the absorbances of the solutions from the Standard Solution and the Test Solution in 1-cm cells at the wavelength of maximum absorbance atabout 575 nm (see Spectrophotometry and Light-Scattering 851), using as the blank the solution from the Purified Water Extracting Medium: the absorbance of the solution from the Test Solution does not exceed that of the solution from the Standard Solution, corresponding to not more than 1 ppm of ethylene glycol.TEST METHODSMultiple Internal ReflectanceApparatus— Use an IR spectrophotometer capable of correcting for the blank spectrumand equipped with a multiple internal reflectance accessory and a KRS-5 internal reflection plate.1 A KRS-5 crystal 2-mm thick having an angle of incidence of 45 provides a sufficient number of reflections.Specimen Preparation— Cut two flat sections representative of the average wall thickness of the container, and trim them as necessary to obtain segments that are convenient for mounting in the multiple internal reflectance accessory. Taking care to avoid scratching the surfaces, wipe the specimens with dry paper or, if necessary, clean them with a soft cloth dampened with methanol, and permit them to dry. Securely mount the specimens on both sides of the KRS-5 internal reflection plate, ensuring adequate surface contact. Prior to mounting the specimens on the plate, they may be compressed to thin uniform films by exposing them to temperatures of about 177 under high pressures (15,000 psi or more).General Procedure— Place the mounted specimen sections within the multiple internal reflectance accessory, and place the assembly in the specimen beam of the IR spectrophotometer. Adjust the specimen position and mirrors within the accessory to permit maximum light transmission of the unattenuated reference beam. (For a double-beam instrument, upon completing the adjustments in the accessory, attenuate the reference beam to permit full-scale deflection during the scanning of the specimen.) Determine the IR spectrum from 3500 to 600 cm–1 for polyethylene and polypropylene and from 4000 to 400 cm–1 for PET and PETG.Thermal AnalysisGeneral Procedure— Cut a section weighing about 12 mg, and place it in the test specimen pan. [N OTE—Intimate contact between the pan and the thermocouple is essential for reproducible results. ] Determine the thermogram under nitrogen, using the heating and cooling conditions as specified for the resin type and using equipmentcapable of performing the determinations as specified under Thermal Analysis 891. For Polyethylene— Determine the thermogram under nitrogen at temperatures between40 and 200 at a heating rate between 2 and 10 per minute followed by cooling at arate between 2 and 10 per minute to 40.For Polypropylene— Determine the thermogram under nitrogen at temperatures ranging from ambient to 30 above the melting point. Maintain the temperature for 10 minutes, then cool to 50 below the peak crystallization temperature at a rate of 10 to 20 per minute.For Polyethylene Terephthalate— Heat the specimen from room temperature to 280at a heating rate of about 20 per minute. Hold the specimen at 280 for 1 minute. Quicklycool the specimen to room temperature, and reheat it to 280 at a heating rate of about 5 per minute.For Polyethylene Terephthalate G— Heat the specimen from room temperature to 120 at a heating rate of about 20 per minute. Hold the specimen at 120 for 1 minute. Quickly cool the specimen to room temperature, and reheat it to 120 at a heating rate of about 10per minute.Biological TestsThe in vitro biological tests are performed according to the procedures set forth under Biological Reactivity Test, In Vitro 87. Components that meet the requirements of the in vitro tests are not required to undergo further testing. No plastic class designation is assigned to these materials. Materials that do not meet the requirements of the in vitro tests are not suitable for containers for drug products.If a plastic class designation is needed for plastics and other polymers that meet the requirements under Biological Reactivity Test, In Vitro 87, perform the appropriate in vivo test specified for Classification of Plastics under Biological Reactivity Test, In Vivo88.Physicochemical TestsThe following tests, designed to determine physical and chemical properties of plastics and their extracts, are based on the extraction of the plastic material, and it is essential that the designated amount of the plastic be used. Also, the specified surface area must be available for extraction at the designated temperature.Testing Parameters—Extracting Medium— Unless otherwise directed in a specific test below, use PurifiedWater (see monograph) as the Extracting Medium, maintained at a temperature of 70 during the extraction of the Sample Preparation.Blank— Use Purified Water where a blank is specified in the tests that follow.Apparatus— Use a water bath and the Extraction Containers as described under Biological Reactivity Tests, In Vivo 88. Proceed as directed in the first paragraph ofPreparation of Apparatus under Biological Reactivity Tests, In Vivo 88. [N OTE—The containers and equipment need not be sterile. ]Sample Preparation— From a homogeneous plastic specimen, use a portion, for each 20.0 mL of Extracting Medium, equivalent to 120 cm2 total surface area (both sides combined), and subdivide into strips approximately 3 mm in width and as near to 5 cm in length as is practical. Transfer the subdivided sample to a glass-stoppered, 250-mL graduated cylinder of Type I glass, and add about 150 mL of Purified Water. Agitate for about 30 seconds, drain off and discard the liquid, and repeat with a second washing.Sample Preparation Extract— Transfer the prepared Sample Preparation to a suitable extraction flask, and add the required amount of Extracting Medium. Extract by heating in。

美国药典USP31-NF26无菌检查法《71》.doc71 STERILITY TESTS 无菌检查法此通则的各部分已经与欧洲药典和/或日本药典的对应部分做了协调。

不一致的部分用符号（）来标明。

下面这些步骤适用于测定是否某个用于无菌用途的药品是否符合其具体的各论中关于无菌检查的要求。

只要其性质许可，这些药品将使用供试产品无菌检查法项下的膜过滤法来检测。

如果膜过滤技术是不适合的，则使用在供试产品无菌检查法项下的培养基直接接种法。

除了具有标记为无菌通道的设备之外，所有的设备均须使用培养基直接接种法进行检测。

在结果的观测与理解项下包含了复验的规定。

由于无菌检查法是一个非常精确的程序，在此过程中程序的无菌状态必须得到确保以实现对结果的正确理解，因此人员经过适当的培训并取得资质是非常重要的。

无菌检查在无菌条件下进行。

为了实现这样的条件，试验环境必须调整到适合进行无菌检查的方式。

为避免污染而采取的特定预防措施应不会对任何试图在检查中发现的微生物产生影响。

通过在工作区域作适当取样并进行适当控制，来定期监测进行此试验的工作条件。

这些药典规定程序自身的设计不能确保一批产品无菌或已经灭菌。

这主要是通过灭菌工艺或者无菌操作程序的验证来完成。

当通过适当的药典方法获得了某物品中微生物污染的证据，这样获得的结果是该物品未能达到无菌检验要求的结论性证据，即便使用替代程序得到了不同的结果也无法否定此结果。

如要获得关于无菌检验的其他信息，见药品的灭菌和无菌保证<1211>按照下面描述的方法配制实验用培养基；或者使用脱水培养基，只要根据其制造商或者分销商说明进行恢复之后，其能够符合好氧菌、厌氧菌、霉菌生长促进试验的要求即可。

使用经过验证的工艺对培养基进行灭菌操作。

下面的培养基已经被证实适合进行无菌检查。

巯基醋酸盐液体培养基主要用于厌氧菌的培养。

但其也用于检测好氧菌。

大豆酪蛋白消化物培养基适合于培养霉菌和好氧菌。

Fluid Thioglycollate Medium 巯基醋酸盐液体培养基将L-胱氨酸、氯化钠、葡萄糖、酵母提取物、酪蛋白胰酶消化物与纯净水混合，并加热至实现溶解。

【关键字】标准232元素杂质—限度介绍本通则明确了药品中各元素杂质的限度。

元素杂质包括催化剂、环境污染物，可能存在于原料药、赋形剂、制剂中。

这些杂质或自然产生，或有意添加，或由于不注意而引入（例如，与处理设备相互作用）。

当知道元素杂质存在，或有意添加，或有引入的可能性，应当保证这些杂质符合限度要求。

可以采用基于风险的控制策略来确保产品满足限度标准。

由于砷、镉、铅和汞普遍存在的特性，风险控制策略至少应考虑这四种元素。

不管采用什么分析方法，所有药品均应满足元素杂质限度标准。

本章提出的限度标准不适用于赋形剂与原料药，除非本章或各论中明确说明。

然而赋形剂与原料药中元素杂质水平必须报告。

本章提出的限度标准同样不适用于兽用产品和常规疫苗。

饮食补充剂和它们的成份的相关规定见于《饮食补充剂中的元素杂质》.形态分析对于元素氧化态、有机络合态、化合态的测定，称为形态分析。

每种元素可能存在不同的氧化态或络合态。

然而，砷和汞应特别关注，因为它们的无机态和络合有机态具有不同的毒性。

砷的限度标准是基于无机态（毒性最大）。

假定样品中所有砷都是无机态，可用总砷测定法检测。

当总砷法结果超过限度标准，应当使用能够对不同形态砷定量的分析方法，以确定无机态砷是否满足法定要求。

汞的限度标准是基于无机（2+）氧化态。

甲基汞（毒性最强），但对于药品，通常不是问题。

这样，汞限度标准的确定是基于汞最常见的无机形态。

对于可能含有甲基汞的产品（例如，从鱼中得到的物质），相应的汞限度标准将在各论中提及。

接触途径元素杂质的毒性跟接触程度（生物利用度）有关。

对于每一种元素杂质接触程度取决于给药途径：口服、肠外注射、吸入。

这些限度确定是基于慢性接触。

为建立标准需要，另两种给药途径，黏膜和局部接触可认为跟口服相同，而表1中的PDE值也适用于这些产品[注意—药品的给药途径在制剂通则中介绍制剂通则1151 . ]Change to read:药品表1的第二至第四栏给出的限度值是一些元素杂质的基本日剂量PDE值（病人按指定给药途径服用）。