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建立高效液相色谱法监测牛奶中苯并咪唑类药物残留。

Development of a high-performance liquid chromatography method to monitor the residues of benzimidazoles in bovine milk.

机构信息

MAO Key Laboratory of Food Safety Evaluation/National Reference Laboratory of Veterinary Drug Residues (HZAU), Huazhong Agricultural University, Wuhan, Hubei 430070, PR China.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2010 Oct 15;878(28):2928-32. doi: 10.1016/j.jchromb.2010.08.029. Epub 2010 Sep 20.

Abstract

A reversed-phase high-performance liquid chromatography with ultraviolet (UV) detection was developed that can determine 11 benzimidazole (BZDs) and 10 metabolites of albendazole, fenbendazole and mebendazole in bovine milk. Samples were extracted with acetonitrile and purified by mixed-mode cation exchange (MCX) solid phase extraction cartridges. LC separations were performed on a C(18) column with gradient elution using acetonitrile and ammonium acetate solution. The UV-detection was set at 292nm. The method is very sensitive to each analyte with limits of quantification (LOQs) of lower than 10μgkg(-1). The recoveries of the BZDs and their metabolites spiked in milk were more than 78% with between-day relative standard deviation values less than 16% at the concentration of 10, 50 and 100μgkg(-1). The method developed has been successfully applied to monitoring real samples containing BZDs, which demonstrated that it is a simple, fast and robust method, and could be used as a regulatory toll to determine the residues of BZDs in milk.

摘要

建立了一种反相高效液相色谱-紫外(UV)检测法,可用于检测牛奶中 11 种苯并咪唑(BZDs)和阿苯达唑、芬苯达唑和甲苯咪唑的 10 种代谢物。样品用乙腈提取,并用混合模式阳离子交换(MCX)固相萃取小柱净化。LC 分离在 C(18)柱上进行,采用乙腈和乙酸铵溶液梯度洗脱。UV 检测波长为 292nm。该方法对每种分析物都非常敏感,定量限(LOQs)均低于 10μgkg(-1)。在 10、50 和 100μgkg(-1)浓度下,BZDs 及其代谢物在牛奶中的加标回收率均高于 78%,日内相对标准偏差值小于 16%。该方法已成功应用于监测含有 BZDs 的实际样品,证明该方法简单、快速、稳健,可作为监管手段用于检测牛奶中 BZDs 的残留。

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