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一种简单、低成本且稳健的毛细管区带电泳方法,采用电容耦合无接触电导检测,用于资金有限的实验室常规测定四种选定的青霉素。

A simple, low-cost and robust capillary zone electrophoresis method with capacitively coupled contactless conductivity detection for the routine determination of four selected penicillins in money-constrained laboratories.

作者信息

Paul Prasanta, Sänger-van de Griend Cari, Adams Erwin, Van Schepdael Ann

机构信息

KU Leuven-University of Leuven, Pharmaceutical Analysis, Department of Pharmaceutical and Pharmacological Sciences, Leuven, Belgium.

Analytical Pharmaceutical Chemistry, Uppsala University, Husargatan, Sweden.

出版信息

Electrophoresis. 2018 Oct;39(20):2521-2529. doi: 10.1002/elps.201800033. Epub 2018 May 4.

Abstract

A simple and robust capillary zone electrophoresis method was developed and validated for the determination of amoxicillin and clavulanate, ampicillin, phenoxymethyl penicillin (Pen V) as well as flucloxacillin. Capacitively coupled contactless conductivity detection was employed as detection mode that makes CE a simple and economic tool for money-constrained laboratories. The developed method is straightforward and user-friendly. It offers good sensitivity and sufficient selectivity for the routine assay of the selected penicillins. The repeatabilities were <1.9% RSD for relative peak areas and <1% RSD for migration times for all the analytes. The method showed good linearity (R  > 0.995) within the 80-120% range of the target concentration (0.5 mg/mL) for each antibiotic. The accuracy of the method, evaluated by standard fortification at three levels, was good for all the analytes. An extended robustness study was performed by varying ±10% of the optimum value of TRIS concentration, l-histidine concentration and temperature in a full factorial design at two levels. This was to evaluate larger than usual variability of factors on the assay value, in order to better cover potential global variance in lab conditions and equipment. Finally, the method was applied for the determination of percent (%) content of all antibiotics in available formulations.

摘要

开发并验证了一种简单且稳健的毛细管区带电泳方法,用于测定阿莫西林和克拉维酸、氨苄西林、苯氧甲基青霉素(青霉素V)以及氟氯西林。采用电容耦合非接触式电导检测作为检测模式,这使得毛细管电泳成为资金有限的实验室的一种简单且经济的工具。所开发的方法直接且用户友好。它对所选青霉素的常规测定具有良好的灵敏度和足够的选择性。所有分析物的相对峰面积的重复性RSD<1.9%,迁移时间的重复性RSD<1%。该方法在每种抗生素目标浓度(0.5mg/mL)的80 - 120%范围内显示出良好的线性(R>0.995)。通过在三个水平上进行标准加标评估该方法的准确度,所有分析物的准确度都很好。通过在全因子设计中以两个水平将TRIS浓度、L - 组氨酸浓度和温度的最佳值变化±10%,进行了扩展的稳健性研究。这是为了评估比通常更大的因素变异性对测定值的影响,以便更好地涵盖实验室条件和设备中的潜在总体差异。最后,该方法用于测定市售制剂中所有抗生素的百分含量(%)。

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