Ionic Chrometography
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亲和色谱法affinity chromatography离子交换色谱法ion exchange chromatography,IEC离子色谱法ion chromatography离子抑制色谱法ion suppression chromatography离子对色谱法ion pair chromatography疏水作用色谱法hydrophobic interaction chromatography制备液相色谱法preparative liquid chromatography平面色谱法planar chromatography纸色谱法paper chromatography薄层色谱法thin layer chromatography,TLC高效薄层色谱法high performance thin layer chromatography,HPTLC 浸渍薄层色谱法impregnated thin layer chromatography凝胶薄层色谱法gel thin layer chromatography离子交换薄层色谱法ion exchange thin layer chromatography制备薄层色谱法preparative thin layer chromatography薄层棒色谱法thin layer rod chromatography液相色谱仪liquid chromatograph制备液相色谱仪preparative liquid chromatograph凝胶渗透色谱仪gel permeation chromatograph涂布器spreader点样器sample applicator色谱柱chromatographic column棒状色谱柱monolith column monolith column微粒柱microparticle column填充毛细管柱packed capillary column空心柱open tubular column微径柱microbore column混合柱mixed column组合柱coupled column预柱precolumn保护柱guard column预饱和柱presaturation column浓缩柱concentrating column抑制柱suppression column薄层板thin layer plate色谱图chromatogram色谱峰chromatographic peak峰底peak base峰高h,peak height峰宽W,peak width半高峰宽Wh/2,peak width at half height峰面积A,peak area拖尾峰tailing area前伸峰leading area假峰ghost peak畸峰distorted peak反峰negative peak拐点inflection point原点origin斑点spot区带zone复班multiple spot区带脱尾zone tailing基线base line基线漂移baseline drift基线噪声N,baseline noise统计矩moment一阶原点矩γ1,first origin moment二阶中心矩μ2,second central moment三阶中心矩μ3,third central moment液相色谱法liquid chromatography,LC液液色谱法liquid liquid chromatography,LLC 液固色谱法liquid solid chromatography,LSC正相液相色谱法normal phase liquid chromatography反相液相色谱法reversed phase liquid chromatography,RPLC柱液相色谱法liquid column chromatography高效液相色谱法high performance liquid chromatography,HPLC尺寸排除色谱法size exclusion chromatography,SEC凝胶过滤色谱法gel filtration chromatography凝胶渗透色谱法gel permeation chromatography,GPC亲和色谱法affinity chromatography离子交换色谱法ion exchange chromatography,IEC离子色谱法ion chromatography离子抑制色谱法ion suppression chromatography离子对色谱法ion pair chromatography疏水作用色谱法hydrophobic interaction chromatography制备液相色谱法preparative liquid chromatography平面色谱法planar chromatography纸色谱法paper chromatography薄层色谱法thin layer chromatography,TLC高效薄层色谱法high performance thin layer chromatography,HPTLC 浸渍薄层色谱法impregnated thin layer chromatography凝胶薄层色谱法gel thin layer chromatography离子交换薄层色谱法ion exchange thin layer chromatography制备薄层色谱法preparative thin layer chromatography薄层棒色谱法thin layer rod chromatography液相色谱仪liquid chromatograph制备液相色谱仪preparative liquid chromatograph凝胶渗透色谱仪gel permeation chromatograph涂布器spreader点样器sample applicator色谱柱chromatographic column棒状色谱柱monolith column monolith column微粒柱microparticle column填充毛细管柱packed capillary column空心柱open tubular column微径柱microbore column混合柱mixed column组合柱coupled column预柱precolumn保护柱guard column预饱和柱presaturation column浓缩柱concentrating column抑制柱suppression column薄层板thin layer plate浓缩区薄层板concentrating thin layer plate荧光薄层板fluorescence thin layer plate反相薄层板reversed phase thin layer plate梯度薄层板gradient thin layer plate烧结板sintered plate展开室development chamber往复泵reciprocating pump注射泵syringe pump气动泵pneumatic pump蠕动泵peristaltic pump检测器detector微分检测器differential detector积分检测器integral detector总体性能检测器bulk property detector溶质性能检测器solute property detector(示差)折光率检测器[differential] refractive index detector 荧光检测器fluorescence detector紫外可见光检测器ultraviolet visible detector电化学检测器electrochemical detector蒸发(激光)光散射检测器[laser] light scattering detector 光密度计densitometer薄层扫描仪thin layer scanner柱后反应器post-column reactor体积标记器volume marker记录器recorder积分仪integrator馏分收集器fraction collector工作站work station固定相stationary phase固定液stationary liquid载体support柱填充剂column packing化学键合相填充剂chemically bonded phase packing 薄壳型填充剂pellicular packing多孔型填充剂porous packing吸附剂adsorbent离子交换剂ion exchanger基体matrix载板support plate粘合剂binder流动相mobile phase洗脱(淋洗)剂eluant,eluent展开剂developer等水容剂isohydric solvent改性剂modifier显色剂color [developing] agent死时间t0,dead time保留时间tR,retention time调整保留时间t'R,adjusted retention time死体积V0,dead volume保留体积vR,retention volume调整保留体积v'R,adjusted retention volume柱外体积Vext,extra-column volune粒间体积V0,interstitial volume(多孔填充剂的)孔体积VP,pore volume of porous packing 液相总体积Vtol,total liquid volume洗脱体积ve,elution volume流体力学体积vh,hydrodynamic volume相对保留值ri.s,relative retention value分离因子α,separation factor流动相迁移距离dm,mobile phase migration distance流动相前沿mobile phase front溶质迁移距离ds,solute migration distance比移值Rf,Rf value高比移值hRf,high Rf value相对比移值Ri.s,relative Rf value保留常数值Rm,Rm value板效能plate efficiency折合板高hr,reduced plate height分离度R,resolution液相载荷量liquid phase loading离子交换容量ion exchange capacity负载容量loading capacity渗透极限permeability limit排除极限Vh,max,exclusion limit拖尾因子T,tailing factor柱外效应extra-column effect管壁效应wall effect间隔臂效应spacer arm effect边缘效应edge effect斑点定位法localization of spot放射自显影法autoradiography原位定量in situ quantitation生物自显影法bioautography归一法normalization method内标法internal standard method外标法external standard method叠加法addition method普适校准(曲线、函数) calibration function or curve以上为美瑞泰克公司中国办事处从网上搜集并加以整理的,目的只有一个,就是能让每一个应用色谱分析的朋友能够更方便。
China Pharmacy 2017V ol.28No.18中国药房2017年第28卷第18期Δ基金项目:中国医学科学院与健康科技创新工程系统创新团队基金(No.2016-I 2M-3-010)*主管药师,硕士。
研究方向:药品质量标准。
电话:010-********。
E-mail :***************.cn#通信作者:主任药师。
研究方向:药品质量标准。
电话:010-********。
E-mail :****************.cn 枸橼酸芬太尼(Fentanyl citrate )是人工合成的强效麻醉性镇痛药,为阿片类受体激动药,镇痛作用机制与吗啡相似,作用强度为吗啡的60~80倍;其可用于麻醉前、中、后的镇静与镇痛,以及各种肿瘤疼痛和慢性疼痛的治疗[1]。
枸橼酸(柠檬酸)作为枸橼酸芬太尼中的反离子配基,提高了药物的溶解性、稳定性和生物利用度,检测和控制枸橼酸芬太尼原料药和注射液中枸橼酸的含量对保证其结构均一和质量可靠具有积极意义[1]。
目前用于有机酸分析的方法主要有薄层色谱法(TLC )[2-3]、气相色谱法(GC )[4-5]、毛细管电泳法(CE )[6-7]、高效液相色谱法(HPLC )[8-11]和离子色谱法(IC )[12-15]等。
TLC 、GC 和CE 法检测结果不准确,而HPLC 法多采用有机相与一定浓度的缓冲盐溶液洗脱,流动相的制备较为复杂。
IC 法流动相简单,环保无污染;采用在线淋洗液发生器能够简化操作,增强方法重复性;且采用电导或紫外检测器,有较好的选择性和灵敏度[16]。
鉴于此,本课题组采用IC 法建立了测定枸橼酸芬太尼原料药和注射液中枸橼酸含量的方法,以期为其质量控制提供参考。
1材料1.1仪器Thermo Dionex ICS-5000+型IC 仪,包括自循环模式的抑制型电导检测器、EGC-500淋洗液自动发生器、Chromeleon 7.2色谱工作站(美国Thermo Fisher Scientific 公司);XP 205型十万分之一电子分析天平(瑞士Mettler-Toledo 公司);Milli-Q Integral 型超纯水器(德国Merck Millipore 公司)。
气相色谱基本知识1色谱法 chromatography 又称色层法、层析法,是一种对混合物进行分离、分析的方法。
1903年俄国植物学家茨威特在分离植物色素时,得到了各种不同颜色的谱带,故得名色谱法。
以后此法虽逐渐应用于无色物质的分离,但“色谱”一词仍被人们沿用至今。
色谱法的原理是基于混合物中各组分在两相(一相是固定的称为固定相,另一相是流动的称为流动相)中溶解、解析、吸附、脱附,或其它作用力的差异,当两相作相对运动时,使各组分在两相中反复多次受到上述各作用力作用而得到互相分离。
2气相色谱法 gas chromatography,GC 以气体作为流动相的色谱法。
根据所用固定相状态的不同,又可分为气-固色谱法和气-液色谱法。
前者用多孔型固体为固定相,后者则用蒸气压低、热稳定性好、在操作温度下呈液态的有机或无机物质涂在惰性载体上(填充柱)或涂在毛细管内壁(开口管柱)作为固定相。
气相色谱法的优点是:分析速度快,分离效能高,灵敏度高,应用范围广,选择性强,分离和测定同时进行。
其局限性在于不能用于热稳定性差、蒸气压低或离子型化合物等的分析。
3反气相色谱法 inverse gas chromatography (IGC) 反气相色谱法是以被测物质(如聚合物样品)作为固定相,将某种已知的挥发性低分子化合物(探针分子)作为样品注入汽化室,汽化后由载气带入色谱柱中,探针分子在气相和聚合物相两相中进行分配,由于聚合物的组成和结构的不同,与探针分子的作用也就不同,选择合适的检测器,检测探针分子在聚合物相中的保留值,藉此研究聚合物与探针分子以及聚合物之间的相互作用参数等。
在高聚物的研究中得到广泛的应用。
气相色谱法的原理和计算公式等均适用于反气相色谱法。
4超临界流体色谱法 supercritical fluid chromatography 以超临界流体作为流动相(固定相与液相色谱类似)的色谱方法。
超临界流体即为处于临界温度及临界压力以上的流体,它具有对分离十分有利的物化性质,其扩散系数和黏度接近于气体,因此溶质的传质阻力较小,可以获得快速高效的分离,其密度和溶解度又与液体相似,因而可在较低的温度下分析沸点较高、热稳定性较差的物质。
地理专业词汇英语翻译(56)地理专业词汇英语翻译(56)地理专业词汇英语翻译(56)ion concentration 离子浓度ion counter 离子计数管ion effect 离子效应ion exchange 离子交换ion exchange adsorption 离子交换吸附ion exchange capacity 离子交换容量ion exchange chromatography 离子交换色层法ion exchange method 离子交换法ion exchange reaction 离子交换反应ion exchange separation 离子交换分离ion exchange surface 离子交换表面ion exchanger 离子交换剂ion hydration 离子水化ion migration 离子移动ion pair 离子对ion product 离子积ion substitution 离子取代ionic activity 离子活度ionic bond 异极键ionic compound 离子化合物ionic current 离子电流ionic diffusion 离子扩散ionic equilibrium 离子平衡ionic lattice 离子晶格ionic micelles 离子胶束ionic migration 离子移动ionic mobility 离子迁移率;离子迁移率ionic polarization 离子极化ionic potential 离子势ionic radius 离子半径ionic reaction 离子反应ionization 电离化ionization anemometer 电离风速计ionization constant 电离常数ionization of atmosphere 大气电离ionization potential 电离势ionized atom 电离原子ionizing energy 电离能ionosphere 电离圈iridescent clouds 虹彩云iridosmine 铱锇矿iron 铁iron age 铁票代iron bacteria 铁化菌iron beidellite 铁贝得石iron concretion 铁结核iron deficiency anemia 缺铁性贫血iron deposit 铁矿床iron hat 铁帽iron humus ortstein 铁腐殖质硬磐iron lateritic soil 铁质砖红壤土iron manganese concretion 铁锰结核iron meteorite 铁陨石iron ore 铁矿iron ore deposit 铁矿床iron pan 铁盘iron phosphate 磷酸铁iron pollution 铁污染irradiance 辐照度irradiation 照射irreversibility 不可逆性irreversible adsorption 不可逆吸附irreversible gel 不可逆凝胶irreversible process 不可逆过程irrigable culture 灌溉栽培irrigated farming 灌溉农业irrigated land 灌溉地irrigated soil 灌溉土壤irrigation 灌溉irrigation basin 灌溉盆地irrigation canal 灌溉渠irrigation district 灌区irrigation requirement 灌溉需水量irrigation station 灌水站irrigation storage 灌溉水库irrigation system 灌溉系统irritabillity 应激性irritation 刺激isallobar 等变压线isanomal 等地平isanomales 等偏线isanomalic 等偏线isanomalous line 等地平isentropic chart 等熵线图island 岛island arc 弧形列岛isoanemons 等风速线isoanomaly curve 等异常曲线isoanth 等花期线isoanthes 等花期线isobar 等压线isobaric chart 等压图isobaric line 等压线isobaric surface 等压面isobath 等深线isobront 雷暴等时线isocenter 等深点isochemical series 等化学岩系isochimene 等冬温线isochiones 等雪线isochiot 等雪高线isochromate 等色线isochromatism 等色性isochrone 等时线;等时水位线isochronism 等时性isochronograph 等时仪isoclinal fold 等斜褶皱isoclinal ridge 等斜脊isoclinal valley 等斜谷isocompound 异构化合物isodenses 等密度曲线isodose chart 等剂量图isodynamic lines 等磁力线isoelectric focusing 等电聚焦isoelectric point 等电点isogeotherm 等地温线isoglacihypse 等冰冻线isogonal line 等偏线isohel 等日照线isohion 等雪线isohyet 等降水量线isohyetal map 雨量分布图isohygraomen 等湿度线isohygrotherm 等水温线isohypse 等高线isolated hill 孤山isolation 隔离isoline 等值线isoline map 等值线图isoline method 等值线法isolux curve 等照度曲线isomer 异构体isometric granular texture 等粒状结构isometric latitude 等量纬度isometric system 等轴晶系isometric view 等距视图isomorphism 类质同象isomorphous element 同形元素isomorphous replacement 同晶替代isoneph 等云量线isopachous line 等厚线isopachous lines 等厚线isopachous map 等厚线图isopachytes 等厚线isopectic 等冰冻线isopectic lines 等冰冻线isophcnic 等密的isophene 等物候线isopic facies 同相isopiestic line 等压线isopleth 等值线isopleth graph 等值线统计图isoseismal line 等震线isostasy of earth's crust 地壳均衡说isostatic compensation 均衡补偿isostatic deformation 等压变形isostatic reduction 地壳均衡改正isostatic surface 等压面isostatic theory 均衡论isotache 等速线isotaches 等风速线isothere 等暑线isothermal adsorption 等温吸附isothermal atmosphere 等温大气isothermal change 等温变化isothermal layer 等温层isothermal line 等温线isothermal remanent magnetization 等温剩余磁化isothermal surface 等温面isothermobaths 等水温线isothermy 等温isotope 同位素isotope balance 同位素平衡isotope chart 同位素表isotope dosimetry 同位素剂量测定isotope effect 同位素效应isotope geochemistry 同位素地球化学isotope ratio 同位素比isotope separation 同位素分离isotope shift 同位素移动isotope structure 同位素结构地理专业词汇英语翻译(56) 相关内容:。
离⼦交换⾊谱(ion exchange chromatography)2、离⼦交换⾊谱(ion exchange chromatography)蛋⽩质、多肽均属于两性电解质,在缓冲液pH⼩于其等电点时,带净正电荷,⽽在缓冲液pH⼤于其等电点时,带净负电荷。
阴离⼦交换凝胶本⾝带有正电荷基团,阳离⼦交换凝胶本⾝带负电荷基团。
由于静电相互作⽤⽽使样品结合到凝胶上,再采⽤盐浓度梯度或者更换缓冲液的pH值进⾏洗脱对于等电点⼩于5.0的酸性蛋⽩质,推荐使⽤阴离⼦交换,对于等电点⼤于7.0的碱性蛋⽩质,推荐使⽤阳离⼦交换。
两种模式:⼀种使⽬的蛋⽩结合凝胶,通过梯度洗脱;⼀种使⽬的蛋⽩不结合凝胶,⽽⼤部分杂质结合凝胶,则穿过液中含有⽬的蛋⽩。
column chromatography(柱⾊谱)batch chromatography(批⾊谱)c、疏⽔作⽤⾊谱利⽤蛋⽩质、多肽在⾼盐存在下,可以结合疏⽔凝胶,⽽在盐浓度降低时⼜可以解脱的原理实现分离。
d、亲和⾊谱利⽤蛋⽩质、多肽与某些配基的特异性相互作⽤⽽进⾏分离。
例如:酶-底物,酶-抑制剂,糖蛋⽩-凝集素,抗原-抗体等。
近来发展了⾦属螯合亲和⾊谱,⽤于纯化表⾯含⾊氨酸、酪氨酸、组氨酸等的蛋⽩质以及(His)6-tagged重组蛋⽩。
亲和⾊谱分为特异性亲和⾊谱和组别亲和⾊谱两类。
肝素、凝集素、染料、⾦属螯合亲和⾊谱均为组别亲和⾊谱(同⼀配基可以结合许多种蛋⽩质)。
e、反相⾊谱常⽤于蛋⽩质、多肽的HPLC分析,以及多肽的精细制备分离,分辨率极⾼,可以分离两种仅相差⼀个氨基酸的多肽。
如⾎管紧张素(angiotensin)的⼏个亚型通过反相⾊谱可以很好地分离。
同⼀个样品在同⼀Source 30 RPC柱上进⾏分离,由于⾊谱条件进⾏了改变,⾊谱图截然不同,说明反相⾊谱具有⾼度的选择性。
四、应⽤举例例⼀、⼀种抗HIV gp120单克隆抗体的Fab⽚断(E.coli中表达)分⼦量:50 kD等电点:11表达定位:周质(periplasmic)纯化策略:渗透压休克提取周质,阳离⼦交换去除⼤部分杂质,疏⽔作⽤⾊谱进⼀步去除杂质,最后⽤凝胶过滤分离。
浅谈离⼦⾊谱法测定⽔中四种阴离⼦2019-09-01摘要:离⼦⾊谱是⾊谱法的⼀个分⽀, 与电化学分析⽅法和原⼦吸收法等相⽐较,具有快速、简单、选择性好、灵敏度⾼、准确度好以及同时测定多组分等优点。
本⽂通过实验,对离⼦⾊谱法测定⽔中四种阴离⼦的含量进⾏了探讨。
关键词: 离⼦⾊谱;阴离⼦;测定Abstract: ion chromatography is a branch of chromatography, and electrochemical analysis method and the atomic absorption method, etc, in comparison with rapid, simple, and selective, high sensitivity and accuracy in measuring and good and components, etc. This article through the experiments, the ion chromatography method to determine the content of four kinds of anion in water are discussed.Keywords: ion chromatography; Anionic; determination中图分类号: O462 ⽂献标识码: A ⽂章编号:1 实验部分1.1 仪器离⼦⾊谱仪(瑞⼠万通861),MetrosepASUPP4(4.0mm×250mm)阴离⼦⾊谱柱,METROSEPASUPP4/5Guard阴离⼦保护柱,MSCMⅡ抑制器,抑制型电导检测器,0.45µm滤膜,ICNet2.3⾊谱⼯作站。
1.2 试剂淋洗液:碳酸氢钠-碳酸钠溶液:称取0.5712g碳酸氢钠(NaHCO3)和0.7632g碳酸钠(Na2CO3)溶于4L纯⽔中,配制成1.7和1.8mmol/L的流动相,经过0.45µm滤膜真空抽滤;抑制器所需再⽣液为0.5mol/L硫酸;标准溶液:使⽤有证标准物质(江苏省疾病预防控制中⼼F-、Cl-、NO3-、SO42-分别为1.0、5.0、1.0、1.0mg/ml)配制,Cl-单标溶液:配制5.0、10.0、15.0、20.0、30.0、50.0mg/L氯化物标准系列;混合阴离⼦标准溶液成分分别含F-、Cl-、NO3-、SO42-,所有试剂均⽤电阻率为18.2MΩ的超纯⽔配制。
层析技术(色谱法,Chromatography)概念、分类和操作(3)柱层析的基本装置及基本操作目前,最常用的层析类型是各种柱层析,下面就简述柱层析的基本装置及操作方法,薄层层析的装置和操作将在后面详细讨论。
(1)柱层析的基本装置柱层析的基本装置,如图2-21 。
(2)柱层析的基本操作柱层析的基本操作包括以下一些步骤:①装柱柱子装的质量好与差,是柱层析法能否成功分离纯化物质的关键步骤之一。
一般要求柱子装的要均匀,不能分层,柱子中不能有气泡等。
否则要重新装柱。
首先选好柱子,根据层析的基质和分离目的而定。
一般柱子的直径与长度比为1:10~50,凝胶柱可以选1:100~200。
然后将柱子洗涤干净。
将层析用的基质(如吸附剂、树脂、凝胶等)在适当的溶剂或缓冲液中溶胀,并用适当浓度的酸(0.5~1mol/L)、碱(0.5 ~1mol/L)、盐(0.5~ 1mol/L)溶液洗涤处理,以除去其表面可能吸附的杂质。
然后用去离子水(或蒸馏水)洗涤干净并真空抽气(吸附剂等与溶液混合在一起),以除去其内部的气泡。
关闭层析柱出水口,并装入1/3柱高的缓冲液,并将处理好的吸附剂等缓慢地倒入柱中,使其沉降约3cm 高。
打开出水口,控制适当流速,使吸附剂等均匀沉降,并不断加入吸附剂溶液,吸附剂的多少根据分离样品的多少而定。
注意不能干柱、分层,否则必须重新装柱。
最后使柱中基质表面平坦并在表面上留有2~3cm 高的缓冲液,同时关闭出水口。
②平衡柱子装好后,要用所需的缓冲液 (有一定的pH 和离子强度)平衡柱子。
用恒流泵在恒定压力下走柱子,平衡与洗脱时的压力尽可能保持相同。
平衡液体积一般为3~5倍柱床体积,以保证平衡后柱床体积稳定及基质充分平衡。
如果需要,可用兰色葡聚糖2000在恒压下走柱,如色带均匀下降,则说明柱子是均匀的。
有时柱子平衡好后,还要进行转型处理,这方面的内容将会在离子交换层析中加以介绍。
③加样加样量的多少直接影响分离的效果。
离子色谱检测技术在药品检测领域的应用发布时间:2021-09-14T07:29:12.966Z 来源:《科技新时代》2021年6期作者:孙煜[导读] 特别是对药品中的阴离子、阳离子、有机酸、多糖类等,有着可靠的检测优势。
广西壮族自治区食品药品检验所广西南宁530022摘要:离子色谱技术广泛应用于各大检测领域,具有操作简便、分析速度快、灵敏度高等特点,常用于测定阴、阳离子、糖类物质等。
本文介绍了近年来离子色谱检测技术在药品检测领域的应用,为离子色谱技术在未来药品检测领域的拓展应用提供参考。
关键词:离子色谱;检测;应用离子色谱检测技术(Ion Chromatography, IC)发展于20世纪70年代,是一种建立在离子交换色谱法的基础上的一种高效液相色谱分析技术。
IC有着独特的分离选择性,这使其成为传统液相色谱法的一个重要补充技术。
近几年来不断应用于各种检测领域,其中在药品检测领域的应用也有着很大的进展,特别是对药品中的阴离子、阳离子、有机酸、多糖类等,有着可靠的检测优势。
1 离子色谱技术原理IC是以溶液中的阴离子或阳离子作为检测对象,淋洗液均为酸或碱溶液,常用的阴离子检测淋洗液包括氢氧根体系和碳酸盐体系,阳离子检测淋洗液则多为甲基磺酸。
当被测物质和淋洗液流经色谱柱时,淋洗液中有相同电荷的离子与色谱柱离子交换树脂上解离的离子可以进行可逆交换,在这样的条件下,被测物质就会因交换能力不同而被分离,依次流经检测器,检测器则根据不同的检测原理发出信号,并将信号发送给分析软件进行数据分析[1]。
2 离子色谱技术在药品检测领域的应用离子色谱检测技术在药品检测方面已逐渐有了一席之地,《中国药典》2010年版附录首次新增了离子色谱法及四个采用离子色谱进行检测的品种,在《中国药典》2015年版中离子色谱检测的品种增加至9个,除了采用电导检测器外,还采用紫外检测器[2]。
2.1 阴离子的检测IC中常用的阴离子检测淋洗液体系,包括氢氧根体系(NaOH或KOH)和碳酸盐体系(Na2CO3/NaHCO3),其中又以氢氧根淋洗液体系最为常用。
色谱法(chromatography)概念、特点和分类1903年,俄国科学家M.C.ЦВЕТ首创了一种绿叶中分离多种不同颜色色素成分的方法,命名为色谱法(chromatography),由于翻译和习惯的原因,又常称为层析法。
近百年来,色谱法不断发展,形式多种多样。
50年代开始,相继出现了气相色谱、液相色谱、高效液相色谱、薄层色谱、通透色谱、离子交换色谱、凝胶色谱、亲和色谱、金属螯合色谱等。
几乎每一种色谱法都已发展成为一门独立的生化技术,在生化领域内得到了广泛的应用。
色谱技术因操作较简便,设备不复杂,样品量可大可小,既可用于实验室的科学研究,又可用于工业化生产。
它与光电仪器、电子计算机结合,可组成各种各样的高效率、高灵敏度的自动化分离分析装置。
这充分显示色谱技术的强大生命力,它是近代生物化学发展的关键技术之一。
一、色谱法的概念和特点色谱法是利用混合物中各组分的理化性质的差异(吸附力、溶解度、分子形状和大小、分子极性、分子亲和力等),使各组分以不同程度分布在两个相中,其中一个相叫固定相(stationnary phase),另一相流过此固定相叫作流动相(mobile phase)。
由于各组分受流动相作用产生的推力和受固定相作用产生的阻力的不同,使各组分产生不同的移动速度,使得结构上只有微小差异的各组分得到分离。
再配合相应的光学、电学、电化学和或其他相关检测手段,对各组分进行定性和定量分析。
色谱法是一种物理化学分离分析方法。
它既是一种极好的分离纯化的方法,也是一种进行精确定性、定量分析的方法。
在色谱分析中,通常是根据色谱峰的位置来进行定性分析,根据色谱峰的面积或高度进行定量分析的。
色谱法的特点是:1.具有极高的分辨效力:只要选择好适当的色谱法(色谱类型、色谱条件),它就能很好地分离理化性质极为相近的混合物,如同系物、同分异构体,甚至同位素,这是经典的物理化学分离方法不可能达到的。
2.具有极高的分析效率:一般说来,对某一混合组分的分析,只需几十分钟,乃至几分钟就可完成一个分析周期。
离子交换层析(Ion Exchange Chromatography ,IEC)(2)(2)离子交换剂的电荷基团根据与基质共价结合的电荷基团的性质,可以将离子交换剂分为阳离子交换剂和阴离子交换剂。
阳离子交换剂的电荷基团带负电,可以交换阳离子物质。
根据电荷基团的解离度不同,又可以分为强酸型、中等酸型和弱酸型三类。
它们的区别在于它们电荷基团完全解离的pH 范围,强酸型离子交换剂在较大的pH 范围内电荷基团完全解离,而弱酸型完全解离的pH 范围则较小,如羧甲基在pH小于6时就失去了交换能力。
一般结合磺酸基团(-SO3H),如磺酸甲基(简写为SM)、磺酸乙基(S E)等为强酸型离子交换剂,结合磷酸基团(-PO3H2)和亚磷酸基团(-PO2 H)为中等酸型离子交换剂,结合酚羟基(-OH)或羧基(-COOH),如羧甲基(CM)为弱酸型离子交换剂。
一般来讲强酸型离子交换剂对 H 离子的结合力比Na+离子小,弱酸型离子交换剂对H 离子的结合力比Na+离子大。
阴离子交换剂的电荷基团带正电,可以交换阴离子物质。
同样根据电荷基团的解离度不同,可以分为强碱型、中等碱型和弱碱型三类。
一般结合季胺基团(-N(CH3)3),如季胺乙基(QAE)为强碱型离子交换剂,结合叔胺(-N(CH3)2)、仲胺(-NHCH3)、伯胺(-NH2)等为中等或弱碱型离子交换剂,如结合二乙基氨基乙基(DEAE)为弱碱型离子交换剂。
一般来讲强碱型离子交换剂对 OH-离子的结合力比Cl-离子小,弱酸型离子交换剂对OH-离子的结合力比Cl-离子大。
(3)交换容量交换容量是指离子交换剂能提供交换离子的量,它反映离子交换剂与溶液中离子进行交换的能力。
通常所说的离子交换剂的交换容量是指离子交换剂所能提供交换离子的总量,又称为总交换容量,它只和离子交换剂本身的性质有关。
在实际实验中关心的是层析柱与样品中各个待分离组分进行交换时的交换容量,它不仅与所用的离子交换剂有关,还与实验条件有很大的关系,一般又称为有效交换容量。
阳离子层析英文Ion Exchange ChromatographyIon exchange chromatography is a widely used technique in the field of analytical chemistry. It is particularly effective in the separation and purification of ionic compounds. This article aims to provide an overview of ion exchange chromatography, its principles, and its applications.1. IntroductionIon exchange chromatography is a separation technique based on the interactions between charged ions and a stationary phase. The stationary phase consists of a resin with charged functional groups. As the sample passes through the column, the target ions are selectively retained or released based on their affinity for the functional groups.2. Principles of Ion Exchange ChromatographyThe separation process in ion exchange chromatography is governed by the exchange of ions between the sample solution and the stationary phase. There are two main modes of ion exchange chromatography: cation exchange and anion exchange.2.1 Cation Exchange ChromatographyIn cation exchange chromatography, the stationary phase contains negatively charged functional groups, such as carboxylate or sulfonate. The target cations in the sample interact with these negatively charged sites, resulting in their retention. The retention time of each ion depends on its charge, size, and affinity for the stationary phase.2.2 Anion Exchange ChromatographyAnion exchange chromatography operates on a similar principle to cation exchange, but with positively charged functional groups, such as ammonium or primary amino groups, on the stationary phase. The target anions in the sample are retained through electrostatic interactions.3. Column Selection and OperationSelecting an appropriate column for ion exchange chromatography is crucial for successful separation. Factors to consider include the resin type, particle size, and column dimensions. The choice of elution buffer, pH, and ionic strength also plays a significant role in the separation process.4. Applications of Ion Exchange ChromatographyIon exchange chromatography has a wide range of applications in various fields, including pharmaceuticals, environmental analysis, and biochemistry.4.1 Pharmaceutical IndustryIn the pharmaceutical industry, ion exchange chromatography is commonly used for the purification of protein-based drugs. It enables the separation of a target protein from impurities based on charge differences.4.2 Environmental AnalysisIon exchange chromatography is frequently employed in the analysis of environmental samples, such as water and soil. It allows for the separation and quantification of various ionic species, including heavy metal ions.4.3 BiochemistryIn biochemistry, ion exchange chromatography is used for protein purification, characterization, and analysis. It helps in the separation of proteins based on their differences in charge, facilitating protein identification and downstream analysis.5. Advantages and LimitationsIon exchange chromatography offers several advantages, including high resolution, versatility, and relatively low cost. However, it also has some limitations, such as limited capacity for large biomolecules and sensitivity to pH and salt concentration.6. ConclusionIon exchange chromatography is a valuable technique for the separation and purification of ionic compounds. Its principles, applications, and operational considerations should be carefully understood to achieve reliable and reproducible results. With its wide range of applications, ion exchange chromatography continues to play a crucial role in various scientific disciplines.。
1 Ionic Chrometography1.1 ETP ObjectivePurpose: (Overview of parameter(s) to be measured as well as scope of conclusions test is expected to facilitate)Ionic Chrometography is used as a process qualification. This test isrequired when starting a new assembly line, switching to a newprinted circuit board supplier, changing a pcb supplier processs ormaterials, or moving to a new contract manufacturer. The testshould be performed annually to ensure the CM has maintained thequality of work.Ionic Chromatography measures the amount of ionic contaminationthat is present on the surface of the printed circuit board. Ioniccontamination is a concern due to the relationship between highcontamination levels and failure of the printed circuit board due toelectromigration. The purpose of this document is to define the datacollection procedure, the recommend method of analysis, defining thespecification limits of each ion of concern and finally provide directionon action to take when levels are exceeded.Limitations: (Any qualifications that apply to this test procedure or its results).1.2 Key Parameters & Requirement InputsThe test variables which impact product performance can either be classified as Key Noise Parameters or Key Control Parameters as described below. They may be set as test inputs, recorded for analysis or both as specified for this ETP in the following charts.Key Noise Parameters - A key noise parameter (KNP) is any product usage orinteraction variable which cannot be controlled by design (i.e. voltage, ambienttemperature, water quality, etc.). Note that for the purposes of this test, theparameter may be controlled (i.e. specified as an input below) in order tounderstand the impact of the KNP upon product performance.Key Control Parameters- A key control parameter (KCP) is any product usageor interaction variable which can be controlled by design (dimensions, operatingrange, material, etc.).1.3 Test Equipment and Supplies1.4 Expected Test Duration(Based on average conditions; may vary significantly depending upon lab load)Set-up: 2 hrsTest Procedures: 1 hrPost-test/Cleanup: 0.5 hrDocumentation: 0.5 hrTotal Expected Test Duration: 2 Weeks at Outside Lab1.5 Test SamplesSample Size (Number of samples and/or rationale for sample size selection)5 Raw PCBs directly from incoming inspection at the CM.5 PCBs run through the CM process except conformal coating, without placing anycomponents.Qualification/Preconditioning/Setup (Any test sample preparation, stabilization, preconditioning or certification required before testing)1.6 Test Procedure(Detailed, step-by-step directions for running test including photos/diagrams as appropriate)Ionic Chromatography test procedure is defined per IPC-TM-650 2.3.28.ResultsNote - All test results to include:∙Equipment used to generate data∙Calibration (accuracy) of test equipment∙Resolution of test1.7 Results Interpretation(Includes any pertinent guidelines, limitations or insights needed for interpreting results)Different technology circuit boards have different requirements when being evaluated for contamination. For the purposes of this document the two technology levels of printed circuitboards will be referred to as Tech A and Tech B. The distinctions between the two types of boards are shown in the table.Table of Ions for Ionic Chromatography - Tech A appear below.Chlorides, Bromides, Sulfates and WOC and Total all have both an UCL as well as aMaximum value. The reason is, controlling these values is more critical than the other ions, and thus we need to provide trigger points for earlier correction of issues. Theother ions only have an UCL because being less severe; the intent was not to set a level at which we categorically reject the boards. Data shows that these ions are rarelyexceeded and if so then one or more of the critical values will be exceeded. UCLs were set so that proper corrective action could still be taken without rejection of boards.The following shall occur if any of the maximum values listed above are exceeded:If qualifying a new PCB manufacturer or Contract Manufacturer or a process/materialchange at current supplier, then the qualification is rejected until corrective action areimplemented and proven effective through subsequent testing.If maximum is exceeded during audit testing of current product, than the lot(s) of printed circuit boards associated with the failed board shall be placed into non-conformingmaterial.The following shall occur if any of the upper control limits listed above are exceeded:If qualifying a new PCB manufacturer or Contract Manufacturer or a process/materialchange at current suppliers than the qualification approval can continue provided adetail action plan is presented with completion dates and new test dates to the Business to include the OCE of Electronics. A business decision can be made based onapplication, exposure level of saleable units and supporting test data.If upper control limit is exceeded during audit testing of the current product, than the lot(s) of printed circuit boards associated with the out of control board require a correctiveaction plan presented to the OCE of Electronics.1.8 Failure Modes Exercised/Acceleration Factors/Field Failure Correlation(Includes both performance and reliability failure modes which test may exercise. Subjective failure levels denoted with photos for reference as appropriate. Field correlations used to set subjective failure guidelines as appropriate.)Presence of the materials listed in section 9 is known to influence electromigration in printed circuit boards. This test has no acceleration factor. Possible field failures which could result from failure to comply with this test include electronic shorts, which can cause various faults in the control system.1.9 Nomenclature/Vocabulary(Defines all technical terms, variables and acronyms used in the background)1.10 Background(Related theory, methods and standards used to develop test procedure)Ionic Chromatography test procedure is defined per IPC-TM-650 2.3.28.1.11 Reference(Technical studies, standards, articles, etc., which are related to this ETP) IPC-TM-650 2.3.281.12 Revision History(Includes reasoning for release of current revision, with date and name of person releasing revision)。