Separation of polymxins by micellar electrokinetic capillary chromatography

高效液相色谱法测定化妆品中的8种抗氧化剂孟磊;谢黎霞;苏惠;胡小宁【摘要】To develop an reversed-phase HPLC method for determination of propyl gallate(PG),butylated hydroxyanisole (BHA),butylated hydroxytoluene(BHT),n-octyl gallate(OG),dodecylgallate(DG),nordihydroguaiaretic acid (NDGA), tert-butylhydroquinone(TBHQ)and 2,6-ditertbutyl-4-hydroxy-methylphenol(Ionox-100)in cosmetics. Chromatographic con-ditions included an Waters Sunfire (150 mm×3.9 mm×5 μm)column with a mobile phase of A (water,with 0.5% formic acid by weight)and B (acetonitrile,with 0.5% formic acid by weight),UV detector and detection wave length 280 nm,col-umn temperature maintained at 30 ℃ and flow rate of 0.6 mL/min. The standard curve of 8 antioxidants was linear in the range of 0.1 to10μg/mL,with coefficients of 0.9990 to 0.9998.The method was validated in terms of linearity(r>0.999). This method has advantages of quick,high sensitivity and low cost,and it is applicable to the rapid qualitative and quantitative de-tection for cosmetics.%采用反相高效液相色谱法分别对化妆品样品中可能含有的没食子酸丙酯（PG）、叔丁基对羟基茴香醚（BHA）、2，6-二叔丁基对甲酚（BHT）、没食子酸辛酯（OG）、没食子酸十二酯（DG）、正二氢愈创酸（NDGA）、叔丁基对苯二酚（TBHQ）、2，6-二叔丁基-4-甲氧基苯酚（Ionox-100）等8种抗氧化剂进行检测，色谱条件：色谱柱 Waters Sunfire （150 mm×3．9 mm×5μm），流动相A为水（含质量分数0．5％甲酸），B 为乙腈（含质量分数0．5％甲酸），梯度洗脱，采用紫外检测器，检测波长280nm，柱温30℃。

联吡啶钌体系电致化学发光测定精胺的研究赵丹;赵叙;徐恩宇;杨梅【摘要】基于精胺对Ru(bpy)23+电化学发光的显著增强效应,利用池内停流技术,建立了精胺的电化学发光测定法.本方法具有灵敏度高,线性范围宽和分析速度快的特点.在最优条件下,相对电化学发光值与精胺浓度在5×10-8～5×10-5mol/L范围内呈现良好的线性关系,对5×10-8mol/L浓度的精胺进行11次平行测定,其相对标准偏差为3.03%,检出限为2.31×10-8mol/L.【期刊名称】《广州化工》【年(卷),期】2011(039)008【总页数】3页(P64-65,82)【关键词】电化学发光;精胺;联吡啶钌【作者】赵丹;赵叙;徐恩宇;杨梅【作者单位】辽宁师范大学化学化工学院,辽宁大连116029;辽宁师范大学化学化工学院,辽宁大连116029;辽宁师范大学化学化工学院,辽宁大连116029;辽宁师范大学化学化工学院,辽宁大连116029【正文语种】中文精胺 (spermine,Spm)属多胺类化合物,化学名称为[N,N-双 -3丙氨基 ]-1,4-双胺,广泛存在于真核细胞和原核细胞中,在人体新陈代谢过程中发挥着重要作用[1]。

研究发现,精胺水平与肿瘤增长密切相关[2]。

所以,分析和检测精胺具有极其重要的意义。

精胺的检测方法主要有紫外检测法[3]、荧光检测法[4]、色谱法[5]和电泳法[6-7]等。

电化学发光 (ECL)是利用电解技术在电极表面产生某些氧化还原物质而导致的化学发光,所以该方法具有装置简单、重现性好、可进行原位检测以及高灵敏度和高选择性等优点[8]。

联吡啶钌 [Ru(bpy)2+3]是一种常见的 ECL试剂,由于其在水溶液中具有良好的可逆性和稳定性,在生化分析和生物传感器领域得到了广泛的应用[9]。

本实验研究发现精胺对 Ru(bpy)2+3电化学发光有显著的增强效应,且增强程度与精胺浓度呈线性关系。

液相色谱词汇中英文对照液相色谱词汇中英文对照高效毛细管电泳high-performance capillary electrophoresis归一化法normalization method毛细管等电聚焦capillary isoelectric focusing毛细管等速电泳isotachophoresis毛细管电色谱capillary electrochromatography毛细管电泳capillary electrophoresis毛细管电泳电喷雾质谱联用capillary electrophoresis – electr芯片电泳microchip electrophoresis色谱法chromatography色谱峰chromatographic peak色谱峰区域宽度peak width色谱富集过样samt injection of chromatography色谱工作站chromatographic working station色谱图chromatogram色谱仪chromatograph色谱柱chromatographic column色谱柱column色谱柱切换技术switching column technique毛细管超临界流体色谱法capillary supercritical fluid chromat…毛细管电泳基质辅助激光解吸电离质谱离线检测off-line capillar…毛细管电泳离子分析capillary ion analysis毛细管电泳免疫分析immunity analysis of capillary electropho…毛细管胶束电动色谱micellar electrokinetic chromatography毛细管凝胶电泳capillary gel electrophoresis毛细管凝胶柱capillary gel column毛细管亲和电泳affinity capillary electrophoresis毛细管区带电泳capillary zone electrophoresis毛细管有效长度the effective length of capillary electrophor…间接检测indirect detection间接荧光检测indirect fluorescence detection间接紫外检测indirect ultraviolet detection检测器detector检测器检测限detector detectability检测器灵敏度detector sensitivity检测器线性范围detector linear range阴离子交换剂anion exchanger阴离子交换色谱法anion exchange chromatography，AEC高速逆流色谱法high speed counter—current chromatography高温凝胶色谱法high temperature gel chromatography高效液相色谱—付里叶变换红外分析法high performance liquid ch…高效液相色谱法high performance liquid chromatography高效柱high performance column高压流通池技术high pressure flow cell technique高压输液泵high pressure pump高压梯度high—pressure gradient高压液相色谱法high pressure liquid chromatography阴离子交换树脂anion exchange resin荧光薄层板fluorescent thin layer plate荧光检测器fluorescence detector荧光色谱法fluorescence chromatography迎头色谱法frontal chromatography迎头色谱法frontal method硬（质）凝胶hard gel有机改进剂organic modifier有机相生物传感器Organic biosensor有效峰数effective peak number EPN有效理论塔板数number of effective theoretical plates有效塔板高度effective plate height有效淌度effective mobility淤浆填充法slurry packing method予柱pre—column在线电堆集on—line electrical stacking在柱电导率检测on—column electrical conductivity detection噪声noise噪信比noise –signal ratio增强紫外—可见吸收检测技术UV—visible absorption enhanced det…窄粒度分布narrow particle size distribution折射率检测器refractive index detector，RID真空脱气装置vacuum degasser阵列毛细管电泳capillary array electrophoresis蒸发光散射检测器evaporative light-scattering detector，ELSD整体性质检测器integral property detector正相高效液相色谱法normal phase high performance liquid chro…正相离子对色谱法normal phase ion-pair chromatography正相毛细管电色谱positive capillary electrokinetic chromatog…直接化学离子化direct chemical ionization GC-MS直接激光在柱吸收检测on—column direct laser detection纸色谱法paper chromatography置换色谱法displacement chromatography制备色谱preparative chromatography制备色谱仪preparative chromatograph制备柱preparation column智能色谱chromatography with artificial intelligence质量色谱mass chromatography质量型检测器mass detector质量型检测器mass flow rate sensitive detector中压液相色谱middle—pressure liquid chromatography重建色谱图reconstructive chromatogram重均分子量weight mean molecular weight轴向扩散longitudinal diffusion轴向吸收池absorption pool of axial direction轴向压缩柱axial compression column柱端电导率检测out—let end detection of electrical conductiv…柱负载能力column loadability柱后衍生化post-column derivatization柱老化condition (aging) of column柱流出物(column) effluent柱流失column bleeding柱内径column internal diameter柱前衍生化pro-column derivatization柱切换技术column switching technique柱清洗column cleaning柱容量column capacity柱入口压力column inlet pressure柱色谱法column chromatography柱上检测on—line detection柱渗透性column permeability柱寿命column life柱头进样column head sampling柱外效应extra-column effect柱温箱column oven柱效column efficiency柱压column pressure柱再生column regeneration柱中衍生化on-column derivatization注射泵syringe pump转化定量法trans-quantitative method紫外-可见光检测器ultraviolet visible detector, UV-Vis紫外吸收检测器ultraviolet absorption detector自动进样器automatic sampler自由溶液毛细管电泳free solution capillary electrophoresis总分离效能指标over—all resolution efficiency总交换容量total exchange capacity总渗透体积total osmotic volume纵向扩散longitudinal diffusion组合式仪器系统building block instrument最佳流速optimum flow rate最佳实际流速optimum practical flow rate最小检测量minimum detectable quantity最小检测浓度minimum detectable concentration萃取色谱法extraction chromatography脱气装置degasser外标法external standard method外梯度outside gradient网状结构reticular structure往复泵reciprocating pump往复式隔膜泵reciprocating diaphragm pump微分型检测器differential detector微孔树脂micro-reticular resin微库仑检测器micro coulometric detector微量进样针micro—syringe微量色谱法micro—chromatography微乳液电动色谱microemulsion electrokinetic chromatography微生物传感器Microbial sensor微生物显影bioautography微填充柱micro—packed column微吸附检测器micro adsorption detector微型柱micro—column涡流扩散eddy diffusion无机离子交换剂inorganic ion exchanger无胶筛分毛细管电泳non—gel capillary electrophoresis无孔单分散填料non-porous monodisperse packing无脉动色谱泵pulse-free chromatographic pump物理钝化法physical deactivation吸附等温线adsorption isotherm吸附剂adsorbing material吸附剂活性adsorbent activity吸附平衡常数adsorption equilibrium constant吸附溶剂强度参数adsorption solvent strength parameter吸附色谱法adsorption chromatography吸附型PLOT柱adsorption type porous-layer open tubular colum…吸附柱adsorption column吸光度比值法absorbance ratio method洗脱强度eluting power显色器color-developing sprayer限制扩散理论theory of restricted diffusion线速度linear velocity线性梯度linear gradient相比率phase ratio相对保留值relative retention value相对比移值relative Rf value相对挥发度relative volatility相对灵敏度relative sensitivity相对碳(重量)响应因子relative carbon response factor相对响应值relative response相对校正因子relative correction factor相交束激光诱导的热透镜测量heat lens detection of intersect …相似相溶原则rule of similarity响应时间response time响应值response小角激光散射光度计low—angle laser light scattering photomet…小内径毛细管柱Microbore column校正保留体积corrected retention volume校正曲线法calibration curve method校正因子correction factor旋转薄层法rotating thin layer chromatography旋转小室逆流色谱rotational little-chamber counter—current c…选择性检测器selective detector循环色谱法recycling chromatography压电晶体piezoelectric crystal压电免疫传感器Piezoelectric Immunosensor压电转换器piezoelectric transducer压力保护pressure protect压力上限pressure high limit压力梯度校正因子pressure gradient correction factor压力下限pressure low limit衍生化法derivatization method衍生化试剂derivatization reagent阳离子交换剂cation exchanger阳离子交换色谱法cation exchange chromatography, CEC氧化铝色谱法alumina chromatography样品环sample loop样品预处理sample pretreatment液—液分配色谱法liquid—liquid partition chromatography液-液色谱法liquid-liquid chromatography液滴逆流色谱drop counter-current chromatography液固色谱liquid—solid chromatography液晶固定相liquid crystal stationary phase液态离子交换剂liquid ion exchanger液相传质阻力resistance of liquid mass transfer液相色谱—傅里叶变换红外光谱联用liquid chromatography—FTIR 液相色谱—质谱分析法liquid chromatography—mass spectrometry 液相色谱—质谱仪liquid chromatography—mass spectrometer液相色谱法liquid chromatography液相载荷量liquid phase loading溶剂效率solvent efficiency溶解度参数solubility parameter溶液性能检测器solution property detector溶胀swelling溶质性质检测器solute property detector容量因子capacity factor渗透极限分子量permeation limit molecular weight生物色谱biological chromatography生物特异性柱biospecific column生物自显影法bioautography升温速率temperature rate湿法柱填充wet column packing十八烷基键合硅胶octadecyl silane石墨化碳黑graphitized carbon black示差折光检测器differential refraction detector试剂显色法reagent color—developing method手动进样器manual injector手性氨基酸衍生物GC固定相chiral amino aci d derivatives stat…手性拆分试剂chiral selectors手性固定相chiral stationary phase手性固定相拆分法chiral solid phase separation手性环糊精衍生物GC固定相chiral cyclodextrin der GC手性金属络合物GC固定相chirametal stationary phase in GC 手性流动相chiral mobile phase手性流动相拆分法chiral mobile phase separation手性色谱chiral chromatography手性试剂chiral reagent手性衍生化法chiral derivation method疏溶剂理论solvophobic theory疏溶剂色谱法solvophobic chromatography疏溶剂作用理论solvophobic interaction principle疏水作用色谱hydrophobic interaction chromatography树脂交换容量exchange capacity of resin数均分子量number mean molecular weight双保留机理dual reservation mechanism双活塞往复泵two—piston reciprocating pump双束差分检测器detector of dual-beam difference双柱色谱法dual column chromatography水凝胶hydragel水系凝胶色谱柱aqua—system gel column死区域dead zone死体积dead volume塔板理论方程plate theory equation碳分子筛carbon molecular sieve特殊选择固定液selective stationary phase梯度洗脱gradient elution梯度洗脱装置gradient elution device梯度液相色谱gradient liquid chromatography体积排斥理论size exclusion theory体积排斥色谱size exclusion chromatography体积色谱法volumetric chromatography填充柱packed column填料packing material停流进样stop—flow injection通用型检测器common detector涂层毛细管coated capillary拖尾峰tailing peak拖尾因子tailing factor流动分离理论separation by flow流动相mobile phase流动相梯度eluent gradient流体动力学进样hydrostatic pressure injection流体力学体积hydrodynamic volume流型扩散dispersion due to flow profile脉冲阻尼器pulse damper酶传感器Enzyme sensor酶联免疫传感器Enzyme linked immunosensor酶免疫分析enzyme immnunoassay内标法internal standard method内标物internal standard内梯度inside gradient逆流色谱法counter-current chromatography逆流色谱仪counter current chromatograph凝胶过滤色谱gel filtration chromatography凝胶内体积gel inner volume凝胶色谱法gel chromatography凝胶色谱仪gel chromatograph凝胶渗透色谱gel permeation chromatography凝胶外体积gel interstitial volume凝胶柱gel column浓度梯度成像检测器concentration gradient imaging detector 浓度型检测器concentration detector排斥极限分子量exclusion limit molecular weight排斥体积exclusion volume排阻薄层色谱法exclusion TLC漂移drift迁移时间migration time迁移时间窗口the window of migration time前延峰leading peak前沿色谱法frontal chromatography强碱性阴离子交换剂strong—base anion exchanger强酸性阳离子交换剂strongly acidic cation exchanger切换时间switching time去离子水deionized water全多孔硅胶macro—reticular silica gel全多孔型填料macro—reticular packing material全二维色谱Comprehensive two—dim ensional gas chromatography…全硅烷化去活complete silylanization deactivation溶剂强度solvent strength激光解吸质谱法laser desorption MS，LDMS激光色谱laser chromatography激光诱导光束干涉检测detection of laser-induced light beam I…激光诱导毛细管振动测量laser—reduced capillary vibration det…激光诱导荧光检测器laser—induced fluorescence detector记忆峰memory peak记忆效应memory effect夹层槽sandwich chamber假峰ghost peak间断洗脱色谱法interrupted—elution chromatography间接光度(检测）离子色谱法indirect photometric ion chromato…间接光度（检测）色谱法indirect photometric chromatography减压液相色谱vacuum liquid chromatography键合固定相bonded stationary phase键合型离子交换剂bonded ion exchanger焦耳热joule heating胶束薄层色谱法micellar thin layer chromatography胶束液相色谱法micellar liquid chromatography交联度crosslinking degree阶梯梯度stagewise gradient进样阀injection valve进样量sample size进样器injector聚苯乙烯PSDVB聚硅氧烷高温裂解去活high—temperature pyrolysis deactivation…聚合物基质离子交换剂polymer substrate ion exchanger绝对检测器absolute detector可见光检测器visible light detector可交换离子exchangable ion空间性谱带加宽band broadening in space空穴色谱法vacancy chromatography孔结构pore structure孔径pore diameter孔径分布pore size distribution控制单元control unit快速色谱法high-speed chromatography理论塔板高度height equivalent to a theoretical plate（HETP）理论塔板数number of theoretical plates峰面积peak area峰面积测量法measurement of peak area峰面积校正calibration of peak area峰容量peak capacity固定相stationary phase固定液stationary liquid固定液的相对极性relative polarity of stationary liquid固定液极性stationary liquid polarity固相扩散solid diffusion固相荧光免疫分析solid phase fluorescence immunoassay固有粘度intrinsic viscosity光散射检测器light scattering detector硅胶silica gel硅烷化法silanization硅烷化法silanizing硅烷化载体silanized support过压液相色谱法over pressured liquid chromatography，OPLC 恒流泵constant flow pump恒温操作constant temperature method恒压泵constant pressure pump红色载体red support红外检测器infrared detector红外总吸光度重建色谱图total infrared absorbance reconstruct…化合物形成色谱compound—formation chromatography化学发光检测器chemiluminescence detector化学发光检测器Chemiluminescence detector, SCD化学键合固定相bonded stationary phase化学键合相色谱bonded phase chromatography化学色谱法chemi—chromatography环糊精电动色谱cyclodextrin electrokinetic chromatography环形展开比移值circular development Rf value环形展开法circular development缓冲溶液添加剂buffer additives辉光放电检测器glow discharge detector混合床离子交换固定相mixed-bed ion exchange stationary phase 混合床柱mixed bed column活塞泵piston pump活性activation活性硅胶activated silica gel活性氧化铝activated aluminium oxide基流background current or base current基线baseline基线宽度baseline width基质substrate materials基质隔离技术matrix isolation technique电歧视效应the effect of electrical discrimination电迁移进样electrophoretic injection电渗流electroendosmotic flow电渗流标记物electroendosmotic flow marker电渗流淌度electroendosmotic mobility电泳淌度electrophoretic mobility调整保留时间adjusted retention time调整保留体积adjusted retention volume叠加内标法added internal standard method二极管阵列检测器diode—array detector, DAD二维色谱法two-dimensional chromatography二元溶剂体系dual solvent system反冲洗back wash反吹技术back flushing technique反峰negative peak反离子counter ion反相高效液相色谱法reversed phas e high performance liquid ch…反相离子对色谱reversed phase ion pair chromatography反相离子对色谱法reversed phase ion—pair chromatography反相毛细管电色谱reverse capillary electrokinetic chromatogr…反相柱reversed phase column反应色谱reaction chromatography反圆心式展开anti—circular development反转电渗流reverse electroendosmotic flow范第姆特方程式van Deemter equation仿生传感器Biomimic electrode放射性检测器radioactivity detector放射自显影autoradiography非极性固定相non—polar stationary phase非极性键合相non—polar bonded phase非水系凝胶色谱柱non-aqua—system gel column非水相色谱nonaqueous phase chromatography非吸附性载体non—adsorptive support非线性分流non-linearity split stream非线性色谱non-linear chromatography非线性吸附等温线non—linear adsorption isotherm酚醛离子交换树脂phenolic ion exchange resin分离－反应－分离展开SRS development分离数separation number分离因子separation factor分离柱separation column分配等温线distribution isotherm分配色谱partition chromatography分配系数partition coefficient分析型色谱仪analytical type chromatograph分子扩散molecular diffusion封尾endcapping峰高peak heightpH梯度动态分离dynamic separation of the pH gradient pH值梯度洗脱pH gradient elutionZata电势Zata potentialZ形池Z—form pool氨基键合相amino-bonded phase氨基酸分析仪amino acid analyzer安培检测器ampere detector白色载体white support半微柱semimicro—column半制备柱semi-preparation column包覆型离子交换剂coated ion exchanger包覆型填料coated packing material保护柱guard column保留间隙retention gap保留时间retention time保留体积retention volume保留温度retention temperature保留值定性法retention qualitative method保留值沸点规律boiling point rule of retention保留值碳数规律carbon number rule of retention保留指数retention index保留指数定性法retention index qualitative method背景电导background conductance苯酚磺酸树脂phenol sulfonic acid resin苯乙烯styrene比保留体积specific retention volume比例阀proportional valve比渗透率specific permeability比移值Rf value便携式色谱仪portable chromatograph标准偏差standard deviation表观电泳淌度apparent electrophoretic mobility表观交换容量apparent exchange capacity表面电位检测器surface potential detector表面多孔硅胶superficially porous silica gel表面多孔填料superficially porous packing material表面多孔型离子交换剂superficially porous ion-exchanger玻璃球载体glass beads support不分流进样splitless sampling参比柱reference column场放大进样electrical field magnified injection场流分离field—flow fractionation场流分离仪field-flow fractionation场效应生物传感器Field effect transistor based Biosensor常压液相色谱法common-pressure liquid chromatography超声波脱气ultrasonic degas程序变流色谱法programmed flow (gas) chromatography程序升温进样programmed temperature sampling程序升温色谱法programmed temperature （gas）chromatography 程序升温蒸发器programmed temperature vaporizer ，PTV程序升压programmed pressure大孔树脂macro—reticular resin大孔填料macro-reticular packing material大内径毛细管柱Megaobore column单活塞往复泵single piston reciprocating pump单相色谱仪single phase chromatograph单向阀one-way valve单柱离子色谱法single column ion chromatography等度洗脱isocratic elution等离子体色谱法plasma chromatography等途电泳-毛细管区带电泳耦合进样isotachophoresis injection—c…低负荷柱low load column低容量柱low capacity column低压梯度low—pressure gradient低压液相色谱low—pressure liquid chromatography电导池conductance cell电导检测法conductance detection电荷转移分光光度法charge transfer spectrophotometry电化学检测器electrochemical detector电解抑制器electrolyze suppressor。

黄酒中生物胺的分析研究谢铭【摘要】采用丹磺酰氯为衍生试剂,建立了反相高效液相色谱法同时测定腐胺、尸胺、酪胺和组胺4种生物胺的方法,色谱条件为:C18色谱柱分离,甲醇和0.1%乙酸溶液为流动相梯度洗脱,流速0.8 ml/min,二极管阵列检测器,检测波长为254 nm.以1,7-二氨基庚烷为内标.给定条件下4种生物胺得到了较好的分离,线性相关性良好(r＞0.998).腐胺、尸胺和酪胺的检测限为0.8μg/mL,组胺为4 μg/mL.检测方法具有良好的重现性和回收率.在对几种黄酒中生物胺的分析发现4种含有腐胺,3种含有酪胺,各有一种含有组胺和尸胺,最高生物胺含量为435.5 μg/g.【期刊名称】《广州化工》【年(卷),期】2010(038)004【总页数】3页(P139-141)【关键词】高效液相色谱法;生物胺;丹磺酰氯;黄酒【作者】谢铭【作者单位】杭州新力环境工程有限公司,浙江,杭州,310009【正文语种】中文生物胺 (Biogenic Amines,BA)是指一类含氮的脂肪族、芳香族或杂环类有机化合物,其中脂肪族生物胺包括腐胺、尸胺、精胺、亚精胺等,芳香族包括酪胺、苯乙胺等,杂环类包括组胺、色胺等。

在人和动物机体细胞中,适当含量的生物胺 (组胺、色胺、精胺、尸胺等)在调节生长、增强代谢活力、控制血压、消除自由基等方面具有显著作用[1];酪胺和组胺在人和动物激素介导、多巴胺和羟色胺在中枢神经系统传递方面也具有重要作用。

通常,人们摄入的食品中所含的少量生物胺不会对人体产生影响,而当生物胺积累到一定浓度时便具有潜在的毒性作用,如色胺和β-苯乙胺可导致特定病人的高血压和偏头痛,组胺可导致食源性中毒,造成腹部痉挛、呕吐和腹泻等症状[2-3]。

生物胺广泛存在于各类食品中,如乳酪及奶制品,鱼、肉及其制品,巧克力,酒及各类发酵制品和水果、蔬菜等。

生物胺的含量可以作为食品受污染程度及新鲜度的指标,对食品中的生物胺进行检测和定量对于保证人们的健康饮食和合理判断食品卫生状况具有重要意义。

胶束电动毛细管色谱法测定鼻渊舒口服液中栀子苷含量目的建立胶束电动毛细管色谱法测定鼻渊舒口服液中栀子苷含量的方法。

方法以对乙酰氨基酚为内标，采用未涂层融硅石英毛细管柱（52 cm×50 μm ID，有效长度42 cm），以50 mmol/L硼砂溶液+100 mmol/L十二烷基硫酸钠+15%乙腈为运行缓冲液（pH=10），分离电压25 kV，压力进样0.5 psi×10 s，检测波长238 nm。

结果栀子苷在15.02～320.48 μg/mL范围内线性关系良好（r=0.999 5）；低、中、高浓度样品测定结果的RSD均小于1.77%，中间精密度RSD=2.01%。

鼻渊舒口服液中栀子苷低、中、高浓度样品平均回收率为97.50%，RSD=4.43%，栀子苷的胶束电动毛细管色谱法测定结果与HPLC测定结果相符。

结论本研究建立的胶束电动毛细管色谱法简便、快速、准确度高、精密度好，可用于测定鼻渊舒口服液中栀子苷的含量。

Abstract：Objective To establish a micellar electrokinetic capillary chromatography method for content determination of geniposide in Biyuanshu Oral Liquid. Methods Acetaminophen was used as an internal standard，and the separation was performed on an uncoated fused silica capillary of 52 cm × 50 ?m ID （42 cm effective length）with the separation voltage of 25.0 kV. The running buffer contained 50 mmol/L borax，100 mmol/L sodium dodecyl sulfate and 15% acetonitrile （pH=10）. The sample was injected by pressure （10 s，0.5 psi）and detected at 238 nm. Results Geniposide was in good linearity range of 15.02–320.48 μg/mL （r=0.999 5）. The repeatability （low，medium and high concentration of samples）and intermediate precision assays gave satisfactory RSD values of less than 1.77% and 2.01%，respectively. The average recovery of geniposide in Biyuanshu Oral Liquid was 97.50% and the RSD was 4.43%. The contents of geniposide determined by micellar electrokinetic capillary chromatography were in accordance with the results of HPLC analysis. Conclusion The method is simple，fast，accurate and precise，which can be used for the content determination of geniposide in Biyuanshu Oral Liquid.Key words：Biyuanshu Oral Liquid；geniposide；micellar electrokinetic capillary chromatography；content determination梔子苷为栀子的主要活性成分。

芘从H 2O/DMF 混合溶剂向聚苯乙烯/聚丙烯酸二嵌段共聚物平头胶团增溶(Ⅱ)Ξ赵剑曦ΞΞ,　戴闽光(福州大学化学系,福州350002)摘　要:　混合溶剂水含量强烈影响芘从H 2O/DMF 混合溶剂向聚苯乙烯/聚丙烯酸二嵌段共聚物平头胶团的增溶,随着水含量增加而明显增大了芘和胶团内核PS 间的结合力,促进了芘的增溶。

实验结果表明,增加混合溶剂极性组分是实现有效增溶的一种简便方法。

关键词:　两亲嵌段共聚物;平头胶团;有效增溶;混合溶剂中图分类号:　O63 文献标识码:　A 文章编号:　1008-9357(1999)04-0409-05两亲嵌段共聚物胶团作为油溶性药物载体已显示出良好的应用前景〔1-2〕,正受到高度重视。

将油溶性药物有效地增溶进胶团内核中(即在有限时间内达到大的增溶量)是将胶团作为药物载体的重要步骤。

胶团水溶液增溶通常包含疏水化合物在水中溶解和分子态疏水化合物增溶进入胶团内核两步骤,然而由于疏水化合物在水中的溶解度极低,它们在胶团水溶液中往往难以实现有效增溶。

两亲嵌段共聚物平头(crew 2cut )胶团通常在含少量水的某些有机溶剂中容易生成〔3〕,而疏水化合物在这些混合溶剂中的溶解度很高,因此可望通过研究疏水化合物在混合溶剂中的增溶来寻找实现有效增溶的方法,但迄今未见报导这方面的探索。

我们在前文中给出了从芘(Py )荧光发射谱计算增溶量的方法,并以Py 从H 2O/DMF 混合溶剂向聚苯乙烯/聚丙烯酸二嵌段共聚物(PS 2b 2PAA )平头胶团增溶为例,考察了新方法的适用性〔4〕。

本文进一步报道在这个模型体系中H 2O/DMF 混合溶剂对Py 增溶的影响,以期寻找实现有效增溶的途径。

1　实验部分1.1　实验材料PS -b -PAA 含有500个苯乙烯结构单元和60个丙烯酸结构单元,用阴离子聚合法合成,合成方法见前文〔4〕。

PS 2b 2PAA 的多分散性指数为1.04。

Py :Aldrich 公司,在乙醇中重结晶两次。

手性化合物的拆分技术研究进展摘要本文综述了分离外消旋体的几种主要拆分方法的优缺点及其应用情况。

分别有：化学拆分法、膜拆分法、色谱拆分法以及毛细管电泳拆分法。

关键词：手性物；拆分；外消旋体Technical Progress of Chiral SeparationAbstractThis article reviews separation methods of chiral which include chemical，membranous，chromatographic and electrophoretic methods．Key words：chiral compounds；chiral separation；raceme目前获得手性物的主要方法还是通过拆分外消旋体。

早期的拆分方法主要有机械拆分，结晶拆分以及手性溶剂结晶拆分。

这三种方法都是利用外消旋混合物的两种对应体结晶性能不一样的特点进行分离。

已经有较成熟工业应用，但一次性收率较差，在此不做赘述还是本文综述了今年来手性拆分方法中使用较多的化学拆分法、膜拆分、色谱拆分以及毛细管电泳拆分四种拆分技术。

1化学拆分[1]1.1生成非对映体拆分此方法是利用外消旋混合物与手性试剂反应后生成有不同性质的非対映体，从而利用生成物的不同物理性质（溶解度、蒸汽压、结晶速率等）将其分离，再将分离后的物质分别还原成之前的対映体。

还可以使用拆分剂家族代替单一拆分剂进行拆分，所谓拆分剂家族是指有类似结构的2~3个手性剂拆分剂。

组合拆分提高了产品收率和纯度。

1998年Hulsho F L A等人[2]就使用一定量的（S,S）酒石酸衍生物的拆分剂家族拆分3-（1,4-亚乙基哌啶基）苯甲酸酯和3,4-二笨基四氢吡咯，经过一定处理后，两种対映体的纯度（ee值）分别达到了99%和98%。

如果拆分剂不能和対映体反应，就可以利用拆分剂的空穴与两种対映体之间形成氢键或者范德华力能力的不同，将一种対映体优先包裹以达到分离的目的。