Capillary electrophoresis with electrochemiluminescence detection for the analysis of quinolone drugs and pharmacokinetics study

A novel method for the determination of two quinolone drugs norfloxacin （NOR） and levofloxacin （LVX） was described by capillary electrophoresis with electrochemiluminescence detection. The good relationship （r ≥ 0.9991） between peak area and concentration of analytes was established over two orders of magnitude. The limits of detection （LOD, S/N = 3） in standard solution are 4.8 × 10^-7 mol/L for NOR and 6.4 × 10^-7 mol/L for LVX, respectively. The limits of quantitation （LOQ, S/N = 10） in real human urine samples are 1.2 × 10^-6 mol/L for NOR and 1.4 × 10^-6 mol/L for LVX, respectively. The present method was successfully applied to the determination of NOR and LVX in human urine and the studv of oharmacokinetics of NOR.

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.

Quality Analysis of Herbal Medicine Products Prepared from Herba Sarcandrae by Capillary Electrophoresis with Electrochemical Detection

A capillary electrophoresis with electrochemical detection（CE-ED） method was developed for the quality analysis of herbal medicine products prepared from the same herb of Herba Sarcandrae： Fufang Caoshanhu tablets, Qingrexiaoyanning capsules, and Xuekang oral liquids. Under the optimal analysis conditions, the low detection limit[l.0×10^-7 mol/L（S/N=3）] and the wide linear range（1.0×10^-7-1.0×10^-4 mol/L） were obtained for quality standard compound of isofraxidin. The precisions of the peak current and the migration time（as RSDs） for the real sample analysis were 2.0%-2.6%, and 1.2%-1.8% for isofraxidin, respectively. The contents of isofraxidin detected were 15.77 μg/tablet, 0.48 mg/capsule, 1.2 mg/ampoule（Jiangxi）, and 0.44 mg/ampoule（Dalian） for Fufang Caoshanhu tablets, Qingrexiaoyanning capsules, and Xuekang oral liquids from different manufacturers, respectively. Quality estimate was conducted by comparing the contents of isofraxidin in the herbal medicine products with the demanded values of Chinese pharmacopeia. In addition, based on their own unique CE-ED profiles（namely, CE-ED electropherograms） the Xuekang oral liquids from the different manufacturers could be easily identified.

Study on the Interaction between Strychnine and Bovine Serum Albumin by Capillary Electrophoretic Frontal Analysis

The protein binding constant, binding sites of the Strychnos alkaloid-strychnine and bovine serum albumin （BSA） was determined by capillary electrophoretic frontal analysis （CE-FA） for the first time. The experiment was carried out in a polyacrylamide-coated fused silica capillary （48.4 cm×50 μm i.d., 38.1 cm effective length） with 20 mmol/L citrate/MES buffer （pH 6.0, ionic strength 0.17）. The applied voltage was 12 kV and detection wavelength was set at 257 nm. The plateau height of the peak was employed to determine the unbound concentration of drug in BSA equilibrated sample solution based on the external drug standard in the absence of protein. The present method provides a convenient, accurate technique for the early stage of drug screening.

Highly sensitive trivalent copper chelate-luminol chemiluminescence system for capillary electrophoresis chiral separation and determination of ofloxacin enantiomers in urine samples

A simple,fast and sensitive capillary electrophoresis（CE） strategy combined with chemiluminescence（CL） detection for analysis of ofloxacin（OF） enantiomers was established in the present work.Sulfonated p-cyclodextrin（β-CD） was used as the chiral additive being added into the running buffer of luminol-diperiodatocuprate（Ⅲ）（K[Cu（HIO6）2],DPC） chemiluminescence system.Under the optimum conditions,the proposed method was successfully applied to separation and analysis of OF enantiomers with the detection limits（S/N=3） of 8.0 nM and 7.0 nM for levofloxacin and dextrofloxacin,respectively.The linear ranges were both 0.010-100 μM.The method was utilized for analyzing OF in urine;the results obtained were satisfactory and recoveries were 89.5-110.8%,which demonstrated the reliability of this method.This approach can also be further extended to analyze different commercial OF medicines.

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.

Rapid Separation and Quantification of Iron in Uranium Nuclear Matrix by Capillary Zone Electrophoresis (CZE)

A method was developed for rapid separation and determination of iron by employing capillary zone elec-trophoresis (CZE) technique with direct UV detection. Iron could be separated from matrix uranium by di-rect injection of dissolved sample solution into capillary using a mixture of 10 mM HCl and 65 mM KCl (pH = 2) as background electrolyte (BGE) at an applied voltage of 15 kV. The developed method has a very high tolerance for the matrix element U (100 mg/mL) and as such may not need prior separation of iron from the matrix. Iron could be separated with better than 95% recovery. The method showed a linear calibration over a concentration range 1-50 ppm of Fe. The migration times for the iron peak were reproducible within 1% for both pure Fe(III) and in presence of matrix uranium (80 mg/mL). The precision (RSD, n = 22) of peak area obtained for 1ppm of iron was 3.5%. The limit of detection (LOD) (3 ) was 0.1 ppm and the ab-solute LOD was 9 × 10-14 g considering the sample injection volume of 1.5 nL. The developed method has been validated by separating and determining iron in two certified reference materials of U3O8. The method was applied for the determination of iron in different uranium based nuclear materials. The CZE method is versatile for routine analysis as it is simple, rapid and has simple sample preparation procedure.

Quick Single Run Capillary Zone Electrophoresis Determination of Active Ingredients and Preservatives in Pharmaceutical Products

The paper deals with the development of a rapid and efficient Capillary Zone Electrophoresis (CZE) method for Quality Control analysis of pharmaceutical preparations containing antihistamines, decongestants, anticholinergic remedies and preservatives. Active ingredients of interest are: ChlorPheniramine Maleate (CPM), DiPhenhydramine Hydrochloride (DPH), Ephedrine hydrochloride (E), Isopropamide Iodide (II), Pheniramine Maleate (PM), Lidocaine hydrochloride (L), Tetracaine hydrochloride (T), Clopamide Hydrochloride (CH), DiHydroErgochristine (DHE), PhenylEphrine hydrochloride (PE) and Acetaminophen (A). Preservatives studied are: MethylParaben (MeP), EthylParaben (EtP), PropylParaben (PrP), ButylParaben (BuP), p-HydroxyBenzoic Acid (p-HBA). All these analytes were separated in a single run using 60 mM tetraborate buffer solution (TBS) pH = 9.2 as a BackGround Electrolyte (BGE) by using an uncoated fused silica capillary of I.D. = 50 mm and applying a voltage of 25 kV in the first part of the electropheretic run (up to 5.8 min) and 30 kV for the remaining time. The hydrodynamic pressurization of the inlet vial was 20 psi at 7.2 min. up to the end of analysis. Total separation time was of 7.5 min. The method was then successfully validated and applied to the simultaneous determination of active ingredients and preservatives. Good repeatability, linearity, and sensitivity were demonstrated. Precision of migration time (tm) was RSD% < 0.53% and of corrected peak area (Ac) was RSD% < 6.15%. The linearity evaluation gave 0.9928 2 1.000. LOD and LOQ, accuracy (recovery) and ruggedness were evaluated for each analyte demonstrating the good reliability of the method. Analyses of some pharmaceutical real samples were performed.

Rapid and Sensitive CZE Method for Quality Control Analysis of Pharmaceuticals Containing Pseudoephedrine, Triprolidine and Paracetamol

A rapid and sensitive CZE (Capillary Zone Electrophoresis) method for pharmaceutical analysis was developed and fully validated. The active compounds: Pseudoephedrine hydrochloride (PSE), Triprolidine hydrochloride (TRI) and Paracetamol (PAR) were separated and quantitatively determined using the tris-borate 30 mM buffer at pH = 9.0 as a Background Electrolyte (BGE). The electrophoretic separation was carried out at 25 kV in an unmodified fused silica capillary of I.D. = 50 μm with a “bubble-cell” for UV detection at 210 nm and 25&deg;C. The separation was reached in about 3 min. After calibration the method was applied for analysis of three commercially available pharmaceutical preparations. The repeatability (RSD%) of migration time (tm) was ranging between 0.47% and 0.90% and of peak areas (A) between 0.63% and 3.64%. The Limit of Detection (LOD) values was of 0.19 μg/mL, 0.31 μg/mL and 0.08 μg/mL for respectively PSE, TRI and PAR. The results obtained in this study showed that the proposed method was useful in routinely analysis of pharmaceuticals.

寡核苷酸药物生物分析方法的研究进展

寡核苷酸药物是具有不同功能化学修饰的DNA或RNA,主要在基因水平上发挥治疗的作用。到目前为止,已经批准16种寡核苷酸药物用于临床治疗,这也导致了人们对寡核苷酸药物生物分析的兴趣日益增加。尤其需要强大的生物分析工具来研究这些药物的质量控制及体内的药代动力学研究。该篇综述总结了液相色谱、毛细管凝胶电泳、杂交酶联免疫吸附技术在检测寡核苷酸药物的优缺点,为该类药物的研究及质量控制提供一定的思路。

对萼猕猴桃多样性分析及其性别鉴定

[目的]对萼猕猴桃是一种新型耐涝营养系砧木,生产中发现雄株作为砧木效果更好,其种质多样性分析可为选育雄性耐涝对萼猕猴桃砧木提供参考。[方法]以62份对萼猕猴桃种质为材料,根据表型性状及7个简单重复序列标记(SSR)基因型进行多样性分析;同时使用性别相关分子标记进行性别鉴定,并观察其中开花的34份对萼猕猴桃的花朵形态以验证标记鉴定结果。[结果]所用62份对萼猕猴桃种质在7个SSR标记位点上共扩增出69个等位基因,平均等位基因数为9.86,有效等位基因数为2~18,平均多态性信息含量(PIC)为0.626,平均观测杂合度(Ho)和期望杂合度(He)值分别为0.994和0.686。性别相关标记共鉴定出雌株18份,雄株43份;根据34份单株的花器官形态鉴定,发现有13份雌株和21份雄株(标记鉴定结果为9份雌株和25份雄株),标记与表型鉴定的一致性为79.14%。[结论]62份对萼猕猴桃种质多样性丰富,结合植株表型性状和DNA标记基因型可有效地鉴定对萼猕猴桃种质,可为进一步选育优良对萼猕猴桃雄性营养系砧木提供工具和材料。

The new approach of standardization of capillary electrophoresis

In this paper, we develope the new standardization methods to eliminate the influence in capillary electrophoresis (CE). The markers were used to determine the basis position and then correct the data of sample by the migration time of standard sample, and make the migration time of samples consistent with the standard sample by the criterion of the marker. The problem of time transition was corrected in this way. Then according to the peak height or peak area of the marker in the sample (peak height was used here) compared with the standard sample, the sample data was zoomed appropriately. The absorbance error was made to be correct.The wavelet de-noise method was also used to make the data smooth and get a good baseline.

毛细管电泳法测定青菜中敌百虫的残留量

建立了一种测定青菜中有机磷农药敌百虫的方法,样品以二氯甲烷提取,活性炭脱叶绿素,毛细管电泳法检测,最低检出限为2×10-6mol L,敌百虫浓度在5×10-5～2×10-6mol L之间,呈现良好的线性关系,r=0.9914,样品加标回收率为90%～102%。

毛细管电泳法检测蜂蜜中残留的抗生素

用毛细管电泳法对 5种常用的抗生素四环素 (TC) ,土霉素 (OTC) ,多西环素 (DOC) ,金霉素 (CTC)和氯霉素 (CP)进行了分离。研究了电泳缓冲液的 pH、不同有机试剂添加剂、温度等因素对抗生素分离的影响。实验结果表明 ,体积分数为 4%的N 甲基吗啡啉的加入可大大改善分离效果。在各自相应的浓度范围内 ,峰面积和样品浓度之间呈现良好的线性关系 ,重现性好。氯霉素的检测极限为 10 μg/L ,四环素、土霉素、多西环素为 2 0 μg/L ,金霉素为 40 μg/L(信噪比 >5 )。该方法成功地应用于蜂蜜中残留抗生素的测定 ,具有操作简单、快速方便、灵敏度及自动化程度高、重现性好等优点 ,是对含抗生素类物质进行痕量分析的好方法。

毛细管电泳用于形态分析

一种元素的生物可给性、环境行为和迁移性在很大程度上取决于它的形态。如不同的键合形式或氧化态 ,因此 ,作为元素物种鉴别和含量测定的形态分析变得越来越重要。毛细管电泳作为一种分离分析技术有许多优点可以满足形态分析的要求。本文从样品的预处理、毛细管电泳的修饰、进样方式。

高效毛细管电泳前沿分析法研究酸性药物那格列奈与人血浆白蛋白的结合

用高效毛细管电泳前沿分析法研究了酸性药物那格列奈与人血浆白蛋白的结合常数、结合位点和结合率。使用未涂层的毛细管柱 (4 0cm× 5 0 μmi.d .;有效柱长 32cm) ,磷酸盐缓冲溶液 (pH 7.4 ,离子强度0 .17)为背景溶液 ,在紫外检测波长 2 14nm、运行电压 18kV和重力进样 10 0s的条件下 ,利用那格列奈谱峰的平台高度和游离药物浓度的良好线性关系 (r>0 .999,n =6 ) ,测定了那格列奈的游离药物浓度。固定药物浓度 (2 0 0 μmol L ,2 5 0 μmol L) ,考察不同的蛋白质浓度对结合的影响 ;固定蛋白质浓度 (10 0 μmol L) ,考察不同的药物浓度对结合的影响。实验数据采用非线性拟和程序进行处理 ,得到了那格列奈的蛋白质结合参数。高效毛细管电泳前沿分析法测定的数据重现性良好 (RSD <2 .5 % ,n =3) ,在药代动力学和药效学研究方面具有简便、准确的优点。

碱性药物与人血清白蛋白结合参数的毛细管区带电泳/前沿分析

将毛细管区带电泳／前沿分析技术用于测定碱性药物ｖｅｒａｐａｍｉｌ（ＶＥＲ）和ｐｒｏｐｒａｎｏｌｏｌ（ＰＲＯ）与人血清白蛋白（ＨＳＡ）平衡体系中结合参数的研究。通过压力进样将药物白蛋白混合液引入石英毛细管电泳柱（３２ｃｍ×５０μｍｉ．ｄ．，聚丙烯酰胺涂渍柱），在ｐＨ值为７．４、离子强度为０．１７的磷酸缓冲液及运行电压为１０ｋＶ的条件下，未结合的碱性药物的浓度可以通过电泳平台峰的高度定量，并且具有良好的线性关系（相关系数ｒ＝０．９９９）。在数据处理过程中成功的采用非线性回归、Ｓｃａｔｃｈａｒｄ方程和Ｋｌｏｔｚ方程３种评价方法，得到了一致的结果。得到的ＶＥＲ和ＰＲＯ与ＨＳＡ的结合参数：结合位点分别是１．２１～１．３０和０．５４～０．６２。

毛细管电泳法测定性保健品中的西地那非

用毛细管电泳法测定了万艾可片剂和两种市售性保健品中的西地那非。以 6 0mmol/L磷酸二氢钠溶液为缓冲溶液 (pH 5 0 ) ,在 35℃ ,30kV的条件下进行测定 ,结果西地那非的质量浓度为 0 0 7g/L～ 1 0 5 g/L时与相应峰面积的线性关系良好 (r =0 9985 ) ;在实际样品中的平均回收率为 97 4 % ;方法的重现性好 ,峰面积的RSD为4 7%。与目前通行的高效液相色谱法测定西地那非的结果相比 ,毛细管电泳方法所测得的结果同样准确可靠 ,而且样品处理简便 ,测试时间短 ,测试成本低 。

记忆缺失性贝类毒素的主要成分——软骨藻酸的毛细管电泳分析

通过萃取、离子交换等技术 ,建立了毛细管电泳 /紫外检测法分析海洋赤潮生物毒素的重要种类之一、记忆缺失性贝类毒素的主要成分软骨藻酸的方法。结果表明 :软骨藻酸在 0 2mg/L～ 5 0mg/L时具有良好的线性关系 ,相关系数r =0 9990 ;方法检出限为 0 0 6 3mg/L(S/N >3)。在 3个添加水平上进行加标回收试验 (n =6 ) ,平均回收率分别为 97 2 4% ,96 92 %和 97 5 5 % ,RSD分别为 2 .74% ,2 .5 9%和 1.95 %。利用该方法对 5种经济贝类样品进行了测定。该方法简单、灵敏、高效、成本低 ,对软骨藻酸的检测和监控具有重要意义。

砷形态分析方法进展

对光谱分析法、高效液相色谱法、毛细管电泳法以及气相色谱法在砷形态分析中的应用进行了评述 ,比较了各种方法的优缺点。引用文献 82篇。