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毛细管电泳法测定血清和药物中的抗组胺药。

Capillary electrophoresis determination of antihistamines in serum and pharmaceuticals.

机构信息

Area de Química Analítica, Departmen oft Q.F.A., E.S.T.C.E., Universitat Jaume I, Campus Riu Sec, 12071 Castelló, Spain.

出版信息

Anal Chim Acta. 2010 May 7;666(1-2):102-9. doi: 10.1016/j.aca.2010.03.041. Epub 2010 Mar 27.

DOI:10.1016/j.aca.2010.03.041
PMID:20433972
Abstract

A capillary electrophoresis (CE) procedure combined with UV detection has proved useful for the quantification of the most frequently prescribed antihistamines corresponding to the ethylendiamine, ethanolamine, propylamine, piperazine and other derivative groups in serum samples and pharmaceuticals. Discussions have focused primarily on the optimisation of the separation conditions by considering the following experimental parameters: pH, pressure injection and voltage; under the criteria of maximum resolution and minimum analysis time. The optimised parameters for the determination of antihistamines were a 24 cm capillary (effective length), UV detection at 214 nm, 20 mM phosphate running buffer at pH 2.0, 2 psi s(-1) injection pressure and 5 kV applied voltage. Under these conditions, the analysis time was below 10 min. The proposed method was validated according to the International Conference on Harmonisation of Technical Requirements for Registration of Pharmaceuticals for Human Use (ICH) guidelines. The limits of detection and quantification were in the ranges of 4-28 and 40-250 ng L(-1), respectively. Intra- and inter-day precision were tested at three different concentrations of the drugs, obtaining RSD values lower than 3% in most cases. The method was robust (RSD<5.6%), simple, specific and suitable for the practical determination of antihistamines in serum samples and pharmaceuticals with high recoveries (95.7-102.9%) without interferences.

摘要

毛细管电泳(CE)程序与紫外检测相结合,已被证明对血清样本和药物中最常开处方的抗组胺药物(对应乙二胺、乙醇胺、丙胺、哌嗪和其他衍生物基团)的定量非常有用。讨论主要集中在通过考虑以下实验参数来优化分离条件:pH 值、压力进样和电压;在最大分辨率和最短分析时间的标准下。确定抗组胺药物的优化参数为 24cm 毛细管(有效长度)、214nm 处的紫外检测、pH 值为 2.0 的 20mM 磷酸盐运行缓冲液、2psi/s 的进样压力和 5kV 的施加电压。在这些条件下,分析时间低于 10 分钟。该方法根据国际人用药品注册技术要求协调会议(ICH)指南进行了验证。检测限和定量限分别在 4-28 和 40-250ng/L 的范围内。在三种不同药物浓度下测试了日内和日间精密度,在大多数情况下获得的 RSD 值低于 3%。该方法具有稳健性(RSD<5.6%)、简单、特异性强,适用于血清样本和药物中抗组胺药物的实际测定,回收率高(95.7-102.9%),无干扰。

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