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液质联用法测定动物组织中的赛拉嗪和 2,6-二甲吡啶

Determination of xylazine and 2,6-xylidine in animal tissues by liquid chromatography-tandem mass spectrometry.

机构信息

Key Lab of Agro-Product Quality and Safety, Inst. of Quality Standards and Testing Technology for Agro-Products, Chinese Academy of Agricultural Sciences, Beijing, 100081, China.

出版信息

J Food Sci. 2013 Jun;78(6):T955-9. doi: 10.1111/1750-3841.12144. Epub 2013 May 6.

DOI:10.1111/1750-3841.12144
PMID:23647632
Abstract

Xylazine is a potent α2-adrenergic agonist used in veterinary medicine for sedation, analgesia, muscle relaxation, and so on. Its residue in animal-derived food may cause the food safety problem. Moreover, the metabolite 2,6-xylidine was reported to be a genotoxic and carcinogenic compound. Therefore, it is necessary to develop a high sensitive method for analyzing xylazine and metabolite residue in animal products. Here, we described a LC-MS/MS method for simultaneous determination of xylazine and 2,6-xylidine in 4 animal tissues: liver, meat, kidney, and fat. The samples were extracted by acetonitrile, and further clean up by hexane. The analysis was performed on a C18 reversed-phase column and API 5000 Triple Quadrupole mass spectrometry with positive electrospray ionization interface operating in the multiple-reaction monitoring mode. For all of the investigated sample matrix, the limit of detection (limit of quantitation) for xylazine and 2,6-xylidine were 0.06 (0.2) and 1.5 (5) μg/kg, respectively, the recoveries were between 63.5% and 90.8%. The precision was within the range of required criteria for method development. The presented method is sensitive and reproducible, and thus suitable for accurate quantification of xylazine and metabolite residue in animal-derived food products.

摘要

水合氯醛是一种在兽医领域中用于镇静、镇痛、肌肉松弛等的强效α2-肾上腺素能激动剂。其在动物源性食品中的残留可能导致食品安全问题。此外,代谢物 2,6-二甲氧基苯乙胺被报道为一种遗传毒性和致癌性化合物。因此,有必要开发一种用于分析动物产品中水合氯醛和代谢物残留的高灵敏度方法。本研究描述了一种 LC-MS/MS 方法,用于同时测定 4 种动物组织(肝、肉、肾和脂肪)中的水合氯醛和 2,6-二甲氧基苯乙胺。样品用乙腈提取,然后用正己烷进一步净化。分析在 C18 反相柱上进行,API 5000 三重四极杆质谱仪采用正电喷雾电离接口,以多反应监测模式运行。对于所有研究的样本基质,水合氯醛和 2,6-二甲氧基苯乙胺的检测限(定量限)分别为 0.06(0.2)和 1.5(5)μg/kg,回收率在 63.5%至 90.8%之间。精密度在方法开发所需标准范围内。该方法灵敏且重现性好,适用于动物源性食品中准确测定水合氯醛和代谢物残留。

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