毛细管电泳电化学法分离检测盐酸克伦特罗、特布他林和沙丁胺醇

建立了毛细管电泳电化学法对盐酸克伦特罗、特布他林和沙丁胺醇进行分离检测。方法采用胶束电泳体系,以铂圆盘为工作电极,考察了检测电位、缓冲液浓度和pH、十二烷基硫酸钠(SDS)浓度、分离电压等因素的影响。3个分离物在10 kV的分离电压、缓冲体系为15 mmol/L(pH 9.0)硼砂+20 mmol/L SDS条件下得到分离。盐酸克伦特罗、特布他林和沙丁胺醇的线性范围分别为2.0～400,3.5～700,5.0～1000μg/L。方法已用于猪肉样品的检测。     

硫酸阿米卡星的毛细管电泳法快速测定

建立了毛细管电泳高频电导法快速测定注射液中硫酸阿米卡星的新方法.考察了缓冲溶液、有机溶剂添加剂以及分离电压和进样条件等因素对分离检测的影响.采用5.0 mmol/L乳酸-30%(体积分数)乙醇缓冲液体系为运行电泳介质,分离电压20.0 kV,在最佳实验条件下,5.5 min内即可实现硫酸阿米卡星的分离检测,硫酸阿米卡星的线性范围为5.00 ～150 mg/L,检出限为1.5 mg/L.     

毛细管电泳非接触电导分离检测金属氧化物纳米粒子

采用毛细管电泳非接触电导检测技术,以碳酸钠-碳酸氢钠为缓冲体系,同时分离测定了纳米二氧化钛和三氧化二铝两种金属氧化物的悬浮粒子.考察了缓冲溶液种类、浓度及pH对分离效果的影响,探讨了激发频率、激发电压对检测信号信噪比的影响.在最佳分离检测条件下,不同粒径的二氧化钛和三氧化二铝悬浮粒子在8 min内可实现完全分离.所选择的最佳条件为:① pH 10.5缓冲溶液为5 mmol·L-1碳酸钠和碳酸氢钠混合溶液;②分离电压20 kV;③进样条件20 kV,6 s;④激发频率460 kHz;⑤交流激发电压4 V(给出最高的S/N比值).     

微流控芯片非接触电导法分离检测5种阳离子

建立了微流控芯片非接触电导法快速分离检测5种常见阳离子的分析方法。考察了缓冲溶液的种类、浓度和pH、添加剂、检测器的激发电压和激发频率等因素对离子分离及检测的影响。根据离子的峰高和信噪比(S/N),研究了非接触电导检测器的激发电压和激发频率对不同阳离子检测的影响规律。以pH 3.8的15 mmol/L精氨酸(Arg)+15 mmol/L酒石酸+2 mmol/L18-冠醚-6+10%(V/V)甲醇作为运行缓冲液,检测器激发电压100 Vp-p、激发频率40 k Hz,可在70 s内实现NH~+_4,K~+,Na~+,Mg~(2+)和Ca~(2+)的分离检测,5种离子的迁移时间重现性RSD均在1.5%以内。结果还表明,非接触电导检测器激发电压和激发频率对5种阳离子检测的影响规律和最佳检测条件基本相同。     

微流控芯片非接触电导法测定感冒药中盐酸伪麻黄碱和氢溴酸右美沙芬

研究了用微流控芯片非接触式电导法分离检测感冒药日夜百服咛片中的两种主要成分盐酸伪麻黄碱和氢溴酸右美沙芬的方法。优化条件为:缓冲液20 mmol/L Tris 20 mmol/L H3BO3(pH=8.0);进样电压300 V;进样时间10.0 s;分离电压3.0 kV。非接触电导检测器激发电压60 V(Vp-p),频率60 kHz。两种成分的线性范围分别为20~1000 mg/L和10~1000 mg/L;检出限分别为10和5.0 mg/L;样品回收率分别为99.3%和97.6%。     

毛细管电泳-电容耦合非接触电导检测法对运动员营养补剂中人体必需支链氨基酸的检测

建立了运动员营养补剂中3种人体必需支链氨基酸(缬氨酸、亮氨酸、异亮氨酸)的毛细管电泳-电容耦合非接触电导检测(CE-C4D)测定方法。通过研究电泳时背景电解质种类、浓度以及电导检测器的激发电压,激发频率等参数的影响,确定最佳的实验条件为采用未涂层熔融石英毛细管(60 cm×75μm,有效长度50 cm),以5.0 mol/L的乙酸为背景电解质;C4D检测器激发电压为40 V,激发频率为600 kHz;运行电压为+15 kV,温度为25℃。3种氨基酸在50.0~1000.0μmol/L范围内线性关系良好,线性相关系数(R2)均大于0.9994,加标回收率在98.6%~105.4%之间,方法的检出限为14.88μmol/L。方法已应用于运动员蛋白营养补剂中的支链氨基酸的测定。     

高效毛细管电泳电导法拆分苯丙氨酸对映体

以未涂层融硅石英毛细管(50 cm×75μm)为分离柱,2 mmol/L NaAc 2 mmol/L HAc 0.5 mmol/LCu2 (pH 4.0)作为电泳运行液,分离电压15 kV,建立了苯丙氨酸对映体的高效毛细管电泳-电导分离检测的方法。对缓冲溶液的种类、浓度、分离电压、有机改性剂等因素对分离的影响进行了讨论,并对拆分机理进行了初步探讨。     

微芯片毛细管电泳快速测定盐酸洛美沙星

采用微芯片毛细管电泳非接触电导检测法快速测定了盐酸洛美沙星胶囊中盐酸洛美沙星的含量。探讨了缓冲液类型、浓度,添加剂种类、浓度及分离电压、进样时间等因素对分离检测的影响。实验采用5.0mmol/L HAc(pH=2.5)+5%乙醇为缓冲溶液,分离电压3.0 kV,在1 min内实现了盐酸洛美沙星的快速分离测定。优化条件下盐酸洛美沙星的线性范围为20.0～250.0μg/mL,检出限为10.0μg/mL(S/N=3),RSD=2.0%,加标回收率为98.6%～103%。     

毛细管电泳非接触电导法测定4种中枢神经系统用药

运用毛细管电泳非接触式电导检测方法对4种中枢神经系统用药-盐酸阿扑吗啡、氢溴酸加兰他敏、富马酸喹硫平、氯氮平的分离进行了研究。考察了电泳介质的种类、浓度、分离电压、进样时间对分离效果的影响,在10 mmol/L三羟基氨基甲烷(Tris)-8 mmol/L柠檬酸(Cit)-20%甲醇的运行缓冲液中,激发电压为60V,激发频率为600kHz,4种药物在15 min内得到了分离。4种药物的线性范围分别为0.97～15.6 mg/L;0.97～15.6 mg/L;0.48～15.6 mg/L和0.97～250 mg/L,检测限为0.32,0.32,0.16和0.32 mg/L。     

毛细管区带电泳法同时测定饲料中西马特罗、盐酸克伦特罗和沙丁胺醇

建立了同时测定饲料中西马特罗、盐酸克伦特罗与沙丁胺醇的毛细管区带电泳-紫外检测方法。考察了实验参数对 分离和检测结果的影响。在最佳实验条件下,在60 mmol/L的柠檬酸-柠檬酸钠运行缓冲液(pH 6.29)中,上述3种物质在8 min内完全分离。西马特罗、盐酸克伦特罗和沙丁胺醇的线性响应范围为0.1~1.0 mg/L,最低检测限(以信噪比为3计)分 别为0.02,0.03和0.02 mg/L。所建立的方法直接用于饲料中西马特罗、盐酸克伦特罗和沙丁胺醇的测定,结果令人满意 。     

Gold nanomaterials based pseudostationary phases in capillary electrophoresis: A brand‐new attempt at chondroitin sulfate isomers separation

In this work, a CE method with bare gold nanorods (GNRs) based pseudostationary phase was developed and applied for the separation of chondroitin sulfate (CS) isomers, CS, and dermatan sulfate (DS). The separation efficiency was investigated by varying the experimental parameters such as concentration and pH of the BGE, separation voltage, internal diameter of capillary, different size, and morphology of gold nanomaterials. Results showed that different size and morphology of gold nanomaterials had different effects on the separation of CS and DS. The best separation of CS and DS was achieved in the BGE composed of aqueous 150 mmol/L (mM) ethylenediamine + 20 mM sodium dihydrogen phosphate + 30% v/v GNRs, pH 4.5, at the separation voltage of ?10 kV. Capillary was 59.2 cm in length (effective length 49 cm), 50 μm id capillary thermostated at 25°C. CE with bare GNRs used as pseudostationary phase was shown to be a suitable technique for the separation of CS and DS mixtures with wider peaks. RSD of migration time and peak area of CS and DS were 0.13, 0.14 and 0.86, 1.07%, respectively.     

Method development and validation for the analysis of didanosine using micellar electrokinetic capillary chromatography

A selective MEKC method was developed for the analysis of didanosine in bulk samples. Successful separation of didanosine from 13 of its potential impurities, derived from the various synthetic preparation procedures, was achieved. As CZE gave poor separation selectivity, MEKC was preferable. The use of EKC allowed achievement of the separation in a significantly shorter time than conventional HPLC. An anionic long-chain surfactant, lithium dodecyl sulfate (LiDS), was used as the pseudostationary phase and sodium tetraborate buffer as the aqueous phase. In order to obtain the optimal conditions and to test the method robustness, a central composite response surface modeling experiment was performed. The optimized electrophoretic conditions include the use of an uncoated fused-silica capillary with a total length of 40 cm and an ID of 50 microm, a BGE containing 40 mM sodium tetraborate and 110 mM LiDS at pH 8.0, an applied voltage of 18.0 kV, and the capillary temperature maintained at 15 degrees C. The method was found to be robust. The parameters for validation such as linearity, precision, and sensitivity are also reported. Three commercial bulk samples were analyzed with this system.     

毛细管区带电泳测定纳米粒子粒径分布的探索

研究了采用毛细管区带电泳测定纳米粒子粒径分布的可能性。在合适的分散条件下,聚苯乙烯(PS)纳米粒子在进样及电泳迁移过程中不发生团聚。通过选择合适的电泳操作条件,PS纳米粒子可以按照粒径大小得到分离,且迁移时间及峰面积的重现性良好。     

Separation and selectivity in micellar electrokinetic chromatography using sodium dodecyl sulfate micelles or Tween 20-modified mixed micelles

The separation and selectivity of eight aromatic compounds ranging from hydrophilic to hydrophobic properties in micellar electrokinetic chromatography (MEKC) using sodium dodecyl sulfate (SDS) micelles or Tween 20-modified mixed micelles were investigated. The effect of different operation conditions such as SDS and Tween 20 modifier surfactant concentration, buffer pH, and applied voltage was studied. The resolution and selectivity of analytes could be markedly affected by changing the SDS micelle concentration or Tween 20 content in the mixed micelles. Applied voltage and pH of running buffers were used mainly to shorten the separation time. Complete separation of eight analytes could be achieved with an appropriate choice of the concentration of SDS micelles or Tween 20-modified mixed micelles. Quicker elution and better precision could be obtained with SDS-Tween 20 mixed micelles than with SDS micelles. The mechanisms that migration order of those analytes was mainly based on their structures and solute-micelle interactions, including hydrophobic, electrostatic, and hydrogen bonding interactions, were discussed.     

毛细管电泳手性选择剂去硫酸基硫酸软骨素C的研究开发及新药西尼地平对映体的拆分

研究开发了一种新型的毛细管电泳多糖手性选择剂去硫酸基硫酸软骨素C,并用于二氢吡啶类药物对映体的分离。建立了新药西尼地平对映体的拆分方法,同时考察了背景电解质pH值、手性添加剂浓度、工作电压等因素对手性分离的影响。优化的背景电解质pH值 为2.50、手性添加剂的质量浓度为30 g/L,工作电压为10 kV。以去硫酸基硫酸软骨素C为毛细管电泳手性选择剂拆分新药西尼地平对映体,操作简单方便,西尼地平两对映体得到了基线分离,分离度达2.01。     

毛细管电泳法测定阿霉素脂质体药物中的微量硫酸根离子

建立了以硝酸钾作为背景电解质测定阿霉素脂质体药物中微量硫酸根离子的毛细管电泳分析法。考察了分离电压、背景电解质、电渗流改性剂浓度、pH值对分离测定的影响。结果表明,当毛细管长度为60 cm(有效长度51.5 cm)、分离电压为~15 kV、缓冲溶液采用20 mmol/L硝酸钾(pH 7.0)、电渗流改性剂采用0.4 mmol/L十六烷基三甲基氯化铵(CTAC)、检测波长为202 nm时,阿霉素脂质体破乳液中硫酸根离子和氯离子在3 min内得到了基线分离,硫酸根离子迁移时间和峰面积的相对标准偏差分别小于0.01%和1.0%,检出限为5 μg/L。用该方法对阿霉素脂质体样品中的微量硫酸根离子进行了分析测定,结果令人满意。     

Analysis of Salvia officinalis plant extracts by capillary electrophoresis

Salvia officinalis (commonly called Sage) and similar plants contain many compounds of pharmaceutical interest and are used as a tea or in various pharmaceutical products. In this work, the use of CE for analysis of aqueous or ethanolic extracts from various Salvia plants has been studied. Especially, several buffers like borate, phosphate, acetate, etc., were examined under different concentrations, pH, separation voltage, injection time, and other parameters to find the optimal separation conditions. The optimization was also performed using experimental design and artificial neural networks. The optimal conditions were: separation voltage +20 kV, 40 mM buffer borate, pH 9.2, injection time 5 s, and UV detection at 280 nm. A new CE method has been developed, validated, and applied to analyze samples of S. officinalis from various countries.     

Rapid enantiomeric separation of polychlorinated biphenyls by electrokinetic chromatography using mixtures of neutral and charged cyclodextrin derivatives

Electrokinetic chromatography with cyclodextrin derivatives (CD-EKC) was used to achieve the rapid enantiomeric separation of chiral polychlorinated biphenyls (PCBs). Thirteen of the 19 chiral PCBs stable at room temperature were individually separated into their two enantiomers by using 2-morpholinoethanesulfonic acid (MES) buffer (pH 6.5) containing carboxymethylated gamma-cyclodextrin (CM-gamma-CD) as pseudostationary phase mixed with beta-cyclodextrin (beta-CD) or permethylated beta-cyclodextrin (PM-beta-CD). Urea was also added to increase the solubility of PCBs and cyclodextrins in the aqueous separation buffer. Several experimental parameters such as the nature, concentration, and pH of the buffer, nature and concentration of the cyclodextrin derivatives used, and the addition of different additives were studied in order to improve the enantiomeric separation. In addition, the effect of some instrumental parameters such as separation temperature and applied voltage was also investigated. PCBs were enantiomerically separated in less than 12 min by using a 50 mM MES buffer (pH 6.5) containing 20 mM CM-gamma-CD, 10 mM beta-CD or 20 mM PM-beta-CD, and 2 M urea at a temperature of 45 degrees C and an applied voltage of 20 kV.     

Enantiomeric Separation of Epinephrine and Salbutamol by Micellar Electrokinetic Chromatography Using β-Cyclodextrin as Chiral Additive

Introduction The development of chiral substances, especially inthe pharmaceutical field, places increasing demands onanalytical methods for the separation of these kinds ofisomers and the chiral purity control of drugs in phar-macokinetic studies. As the enantiomers of epinephrineand salbutamol have different pharmacological andtoxicological characteristics, separation and quantitationof the single enantiomers are required. Analytical methods used so far for the enantiomerseparation inclu…     

Fast Determination of Clenbuterol and Salbutamol in Feed and Meat Products Based on Miniaturized Capillary Electrophoresis with Amperometric Detection

The fast separation capability of a novel miniaturized capillary electrophoresis with an amperometric detection (μCE‐AD) system was demonstrated by determining clenbuterol and salbutamol in real samples. The effects of several factors such as the acidity and concentration of the running buffer, the separation voltage, the applied potential and the injection time on CE‐AD were examined and optimized. Under the optimum conditions, the two β‐agonists could be baseline separated within 60 s at a separation voltage of 2 kV in a 90 mmol/L H₃BO₃‐Na₂B₄O₇ running buffer (pH 7.4), which was not interfered by ascorbic acid and uric acid. Highly linear response was obtained for above compounds over three orders of magnitude with detection limits ranging from 1.20×10^?7 to 6.50×10^?8 mol/L (S/N=3). This method was successfully used in the analysis of feed and meat products with relatively simple extraction procedures.