Study on Conductivity Detection for Capillary Electrophoresis──Design of a new type of miniature conductance cell

A new kind of ndniature conductance cell with thick electrodes was made, which has high resolution, high sensitivity, but no dead volume. A set of capillary electrophoresis device with on-column conductivity detector was assembled. In order to test the performance of this kind of ndni-cell, different kinds of Anni-cells were used to detect Li+, Na+, K+, Ca2+and Mg2+ ions.

Analysis of arecoline in Semen Arecae decoction pieces by microchip capillary electrophoresis with contactless conductivity detection

A new method for the determination of arecoline in Semen Arecae decoction pieces by microchip capillary electrophoresis with contactless conductivity detection （MCE-CCD） was proposed. The effects of various electrophoretic operating parameters on the analysis of arecoline were studied. Under the optimal conditions, arecoline was rapidly separated and detected in 1 rain with good linearity over the concentration range of 20 1500 uM （r2=0.9991） and the detection limit of 5 uM （S/N=3）. The method was used for the analysis of arecoline satisfactorily with a recovery of 96.8 -104%.

Analysis of Glutamic Acid in Cerebrospinal Fluid by Capillary Electrophoresis with High Frequency Conductivity Detection

A rapid method to determine glutamic acid (Glu) in cerebrospinal fluid (CSF) by capillaryelectrophoresis with high frequency conductivity detection (contactless conductivity detection) wasdescribed. The CSF sample was pretreated with silver cation resin to remove high concentration ofCl- ions in CSF. The separation was achieved in the buffer solution of 10 mmol/L Tris and 8mmol/L boric acid at the separation voltage of 20.0 kV. Glu showed linear response in the range of5.0×10-6 to 6.0×10-3 mol/L, the limit of detection was 1.0×10-6 mol/L. The method was used foranalysis Glu in CSF satisfactorily with a recovery of 97.8-98.8%.

Sensitive Determination of Metal Ions in Drinking Water by Capillary Electrophoresis Coupled with Contactless Conductivity Detection Using 18-Crown-6 Ether and Hexadecyltrimethylammonium Bromide as Complexing Reagents

A simple, economical, and sensitive capillary electrophoresis (CE) method integrated with capacitively coupled contactless conductivity detection was developed for the determination of metal ions such as K+, Na+, Mg2+, Sr2+, Ca2+ in drinking water. 18-Crown-6 ether and Hexadecyltrimethylammonium Bromide (CTAB) were employed as complexing reagents. The effects of electrolyte additives, citric acid buffer solution, and other separation conditions of CE were comprehensively investigated and carefully optimized. The best results were obtained in a running buffer solution composed of citric acid (12 mM), 18-crown-6 ether (0.2 mM), and CTAB (0.015 mM) at pH 3.5. Under these conditions, a complete separation of five metal ions was successfully achieved in less than 12 min. The limits of detection for the optimal procedure were determined to be in the range of 0.02 - 0.2 mg·L-1. The repeatability with respect to migration times and peak areas, expressed as relative standard deviations, was better than 2.3% and 5.1%, respectively. Evaluation of the efficiency of the methodology indicated that it was reliable for the determination of metal ions in six different brands of drinking water samples.

Analysis of Amino Acids in a Single Human Red Blood Cell by Capillary Zone Electrophoresis with Intracellular NDA- derivatization and Electrochemical Detection

A novel method for determination of amino acids in individual human red blood cells has been developed. In this method, the derivatization reagents (NDA and CN-) are introduced into living cells by electroporation. After completion of derivatization, the amino acids in a single cell is determined by capillary zone electrophoresis with end-column amperometric detection.

Assay of Histamine in Single Mast Cells by Capillary Zone Electrophoresis with Electrochemical Detection

Capillary zone electrophoresis was employed for the analysis of histamine in single rat peritoneal mast cells using an amperometric detector. In this method, individual mast cells and then 0.02 mol/L NaOH as a lysing solution are injected into the front end of the separation capillary. A cell injector was constructed for easy injection of single cells. Histamine in single mast cells has been identified and quantified.

Chiral Separation of Ibuprofen and Terbutaline by Nonaqueous Capillary Electrophoresis with Conductance Detection

In the nonaqueous N,N -dimethylformamide medium, the chiral drugs ibuprofen and terbutaline were successfully separated with sulfonyl- β -cyclodextrin(s- β -CD) as the chiral selector by capillary electrophoresis with conductance detection. The comparison of the effects of three CDS( β -CD, diethylic- β -CD, sulfonyl- β -CD) on the chiral separation was made and the resolution mechanism was proposed.

Determination of Amino Acids in an Individual Erythrocyteby Capillary Electrophoresis with Intracellular FITC-derivatization and Laser-induced Fluorescence Detection

A novel approach for analysis of amino acids in individual erythrocytes was established. In this method, the derivatization reagent was introduced into the living cells by electroporation. After derivatization, the amino acids in a single cell were determined by capillary electrophoresis with laser-induced fluorescence detection.

Sensitive Determination of Five Priority Haloacetic Acids by Electromembrane Extraction with Capillary Electrophoresis

A method for sensitive determination of five priority haloacetic acids in drinking water has been developed for the first time based on electromembrane extraction(EME)prior to CZE with capacitively coupled contactless conductivity detection(CZE-C^(4)D).The target analytes were extracted from 10 mL of the sample solution(donor phase),through the supported liquid membrane(using a polypropylene membrane supporting 1-octanol),and into 10μL of 50 mmol/L NaAc solution(acceptor phase).The extracted solution was directly analyzed by CZE-C^(4)D without de-rivatization.Several factors that affect separation,detection and extraction efficiency were investigated.Under the optimum conditions,five haloacetic acids(monochloroacetic acid,dichloroacetic acid,trichloroacetic acid,mono-bromoacetic acid,and dibromoacetic acid)could be well separated from other components coexisting in water samples within 23 min,exhibiting a linear calibration over two orders of magnitude(r≥0.9943);the enrichment factors at 430-671 were obtained in a 30 min of extraction,and the limits of detection were in the range of 0.17-0.61 ng/mL.The intraday relative standard deviations for peak areas investigated at 10 ng/mL were between 1.2%and 9.7%for the combined EME-CZE-C^(4)D procedure.This approach offers an attractive alternative to the officially proposed method for purified drinking water analysis,which requires derivatization procedure prior to gas chromatography analysis.

毛细管电泳法测定氧氟沙星及左氧氟沙星在其制剂中的含量

建立制剂中氧氟沙星及左氧氟沙星毛细管电泳高频电导分析法,并用于片剂、滴眼液中氧氟沙星及左氧氟沙星含量的测定。对电泳介质的种类、浓度以及操作电压和进样量等影响因素进行了优化。实验采用5mmol/L乳酸为缓冲溶液,分离电压20.0kV,可在7min内实现对氧氟沙星及左氧氟沙星的分离和检测。在优化实验条件下,氧氟沙星的线性范围0.4～220μg/ml,检出限0.2μg/ml,回收率94.4%～102%;左氧氟沙星的线性范围0.6～200μg/ml,检出限0.3μg/ml,回收率95.4%～102%。

高效毛细管电泳-电导检测对四环素衍生物分离测定的研究

运用毛细管电泳 电导检测方法对 4种四环素衍生物———土霉素 (OTC)、金霉素 (CTC)、强力霉素 (DOC)和四环素 (TC)的分离进行了研究。在 3.5mmol L三羟基氨基甲烷 (Tris) 7.5mmol L柠檬酸 (Cit)pH 4.0的运行缓冲液中 ,4种四环素衍生物在 1 5min内获得完全分离。四环素衍生物的线性范围分别为 5 .0～5 0 0 μg mLOTC ,3.6～ 42 0 μg mLCTC ,4.5～ 470 μg mLDOC和 2 .5～ 40 0 μg mLTC。检测限 (S N =3)分别为OTC 2 .0 μg mL ,CTC 1 .8μg mL ,DOC2 .5 μg mL和TC 1 .0 μg mL。采用本法对实际样品强力霉素片中强力霉素和土霉素片中土霉素进行测定 ,回收率分别为 97.2 %和 96.4%。

毛细管电泳高频电导法测定青风藤药材及制剂中青藤碱的含量

A method based on capillary electrophoresis with a high frequency conductivity detection was developed for the determination of Sinomenine. The key factors for separation and determination were studied and the best analysis conditions were obtained. In the buffer of 2.0 mmol/L HAc-3.0 mmol/L NaAc-10.0% CH 3OH at a separation voltage of 22 kV, Sinomenine in the sample could be separated and detected within 4 min. The linear mass concentration of Sinomenine is in the range of 1.0—36.0 μg/mL, the limit of detection reached 0.20 μg/mL. The method was used for the analysis of Sinomenine in Sinomenium acutum and tablets satisfactorily with a recovery of 96%—102%.

牡丹皮中有效成分丹皮酚的毛细管电泳快速检测新方法

采用毛细管电泳高频电导法对丹皮酚进行了快速分离检测。对电泳介质的种类及浓度、操作电压和进样时间等影响因素进行了优化。最佳条件为：分离介质1．0mmol／LH3BO3-3．0mmol／L三乙胺-10％CH，OH（pH=8．0），分离电压20．0kV，25．0cm位差虹吸进样8．0s。在该条件下。可在4min内实现对丹皮酚的分离检测。线性范围为2．0～105μg／mL，检出限为0．3μg／mL。成功测定了中药牡丹皮中的丹皮酚，回收率达94％～99％。方法简便、快速、灵敏，可用于药物分析。

毛细管电泳-电导法分离检测磺胺嘧啶、磺胺甲嘧啶和磺胺二甲嘧啶

采用毛细管电泳-电导法建立了磺胺嘧啶、磺胺甲嘧啶、磺胺二甲嘧啶3种结构相近磺胺药物的分离检测方法。以2mmol／L磷酸氢二钠-0．6mmol／L磷酸二氢钠为电泳运行液，分离电压＋12kV。上述3种磺胺药物在10min内实现了基线分离。线性检测范围为0．8—100mg／L，检出限为0．2mg／L（S／N=3）。探讨了缓冲溶液的种类、浓度、pH等诸因素对分离检测结果的影响。应用于市售复方磺胺嘧啶片和小儿安散中磺胺药物的含量测定，取得满意结果。

司帕沙星的毛细管电泳高频电导法测定

采用毛细管电泳高频电导法检测了司帕沙星。探讨了缓冲液的种类、浓度、添加剂以及操作电压和进样时间等因素对分离的影响。选择3.0mmol LHAc-5.0%C2H5OH(V V)为电泳介质,分离电压20.0kV,在4min内可实现司帕沙星的分离检测。在优化条件下,司帕沙星的线性范围为6 0～280 0μg mL,检出限为1 9μg mL。在该条件下,片剂中的敷料不干扰测定,可成功测定片剂中的司帕沙星,样品回收率为98.7%～101%。

非水介质毛细管电泳电导检测舒血宁片中槲皮素含量

以甲醇∶水 =70∶3 0的体系为分离介质 ,柠檬酸 三 (羟甲基 )氨基甲烷 (Citricacid Tris)为支持电解质 ,使用电导检测 ,对槲皮素及其制剂舒血宁片进行了毛细管电泳分离检测 ,对电泳介质的种类、浓度、表观pH值以及操作电压和进样时间对分离的影响进行了研讨 ,并对分离检测机理进行了探讨。建立的测定槲皮素的方法的线性范围为 :8.0～ 1 60 .0mg L;峰面积的RSD(n =6)为 1 .7% ,检出限为 1 .0mg L ;样品加标回收率为92 .8%～ 98.2 %。

毛细管电泳法测定紫草中的紫草素

建立了毛细管电泳高频电导法测定紫草药材中左旋紫草素含量的分析方法.以融硅毛细管（150 μm×70 cm）为分离柱,研究了缓冲液的种类、浓度、添加剂种类与添加量、分离电压和进样量等因素对分离和检测的影响,优化选择1.0 mmol/L H3BO3 ＋ 3.0 mmol/L 三乙胺缓冲液为电泳介质,分离电压18.0 kV,可实现分离检测.在优化条件下左旋紫草素线性范围为10.0～250 mg/L;线性相关系数为0.9962;检出限为5.0 mg/L（S/N=3）.2批样品不同浓度添加水平的日内和日间RSD均小于4%,两批药材的加标回收率分别为93.9%～97.4%和 93.1%～101% .该方法简便、快速、灵敏度高,可以用于紫草药材的质量控制.

高效毛细管电泳电导法快速检测复方维生素B片中的VB_1、VB_(12)、VB_6和VC

采用高效毛细管电泳电导法同时分离、测定了复方维生素B片中的主要成分VB1,VB12,VB6和VC的含量。研究了运行缓冲溶液的酸度和浓度、电泳电压、进样时间等因素对电泳的影响。在优化的实验条件下:40mmol/LTris 4mmol/LH3BO3(pH8.0)的缓冲溶液中加入0.30mmol/LCTAB(溴化十六烷基三甲基铵),分离电压为15kV,上述4组分在5min内得到良好的分离。维生素B1,B12,B6和VC的线性范围分别为5.5～1.0mg/mL;15～1.5mg/mL;1.0～0 40mg/mL和6.6～0.80mg/mL;检测限分别为0.80μg/mL,4.0μg/mL,0.50μg/mL,2.9μg/mL;5次测定峰高的相对标准偏差分别为2.2%,1.6%,3.9%,2.8%。5次测定的平均回收率分别为99%,94%,100%,97%。

毛细管电泳高频电导法测定几种中药中的丁香酚

A method based on capillary electrophoresis with a high frequency conductivity method was(developed) for the determination of eugenol in several Chinese herbal medicines from different producing areas.In this study,some key factors for separation and detection were studied and the best analysis conditions were obtained.In the buffer system of 2.0 mmol/L triethylamine +0.74 mol/L methanol at separation potential of 18.0 kV,the optimal separation and detection was obtained.Under the chosen conditions,eugenol was eluted within 7 min.The linear range of eugenol was 2.0—540 μg/mL,the limit of detection was 0.6 μg/mL,and the recovery ranged from 93.3% to 106%.

毛细管电泳法快速测定复方地芬诺酯片中的地芬诺酯和阿托品

建立了毛细管电泳高频电导法同时测定地芬诺酯和阿托品的方法.探讨了缓冲溶液、有机溶剂添加剂、分离电压和进样条件以及毛细管内径和长度等因素对分离检测的影响.在电泳介质为10.0 mmol/L乳酸-15.0%C2H5OH、分离电压20.0 kV的优化条件下,6 min内即可实现地芬诺酯和阿托品的同时分离检测,线性范围分别为5.00～500和2.00～320 mg/L;检出限分别为3.0和1.0 mg/L.