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基于分散固相萃取的液相色谱-串联质谱法快速检测饲料中授权/禁用环多聚肽类抗生素的多残留分析。

Rapid multiresidue analysis of authorized/banned cyclopolypeptide antibiotics in feed by liquid chromatography-tandem mass spectrometry based on dispersive solid-phase extraction.

机构信息

National Reference Laboratory of Veterinary Drug Residues (SCAU), College of Veterinary Medicine, South China Agricultural University, Guangzhou, 510642, China.

Guangdong Provincial Key Laboratory of Veterinary Pharmaceutics Development and Safety Evaluation, South China Agricultural University, Guangzhou, 510642, China.

出版信息

J Pharm Biomed Anal. 2019 Jun 5;170:234-242. doi: 10.1016/j.jpba.2019.03.050. Epub 2019 Mar 26.

DOI:10.1016/j.jpba.2019.03.050
PMID:30939416
Abstract

An effective analytical strategy was developed for simultaneous determination of seven cyclopolypeptide antibiotics (vancomycin, polymyxin B, polymyxin E, teicoplanin A2, bacitracin A, daptomycin and virginiamycin M1) in feed using liquid chromatography-tandem mass spectrometry. The extraction of sample was based on acidified methanol-aqueous solution, followed by a simply dispersive solid-phase extraction for further purification with primary secondary amine as an adsorbent. The method showed good linearity for target analytes in the experimental concentration ranges. At three spiked concentration levels of 50, 100 and 200 μg/kg, the average recoveries for target compounds were in the range of 63.1%-107.5% with the relative standard deviations less than 14.7%. Matrix effects in different feeds were evaluated and the strong signal suppression (>50%) was observed. Compared with the corresponding methods in literature, the developed method is more economical, more sensitive and involves the detection of authorized/banned cyclopolypeptides in animal feed. The proposed method was successfully applied to the routine supervision and rapid screening of cyclopolypeptide antibiotics in complete and premix feed.

摘要

建立了一种同时测定饲料中七种环多肽抗生素(万古霉素、多粘菌素 B、多粘菌素 E、替考拉宁 A2、杆菌肽 A、达托霉素和维吉尼亚霉素 M1)的高效液相色谱-串联质谱分析方法。样品提取基于酸化甲醇-水溶液,然后用伯仲胺作为吸附剂进行简单分散固相萃取进一步净化。该方法在实验浓度范围内对目标分析物表现出良好的线性。在 50、100 和 200μg/kg 三个加标浓度水平下,目标化合物的平均回收率在 63.1%-107.5%之间,相对标准偏差小于 14.7%。评估了不同饲料中的基质效应,观察到强烈的信号抑制(>50%)。与文献中的相应方法相比,该方法更经济、更灵敏,并涉及到对动物饲料中授权/禁用的环多肽的检测。该方法成功应用于全价和预混料饲料中环多肽抗生素的常规监测和快速筛选。

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