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超高效液相色谱-串联质谱法测定牛组织中伊维菌素残留的高灵敏度定量/确证方法的建立与验证

Development and validation of a highly sensitive quantitative/confirmatory method for the determination of ivermectin residues in bovine tissues by UHPLC-MS/MS.

作者信息

Hoyos O Duvan E, Cuartas O Yudy A, Peñuela M Gustavo A

机构信息

GDCON Research Group, Faculty of Engineering, University Research Headquarters (SIU), University of Antioquia, Street 70 # 52-21, Medellin, Colombia.

GDCON Research Group, Faculty of Engineering, University Research Headquarters (SIU), University of Antioquia, Street 70 # 52-21, Medellin, Colombia.

出版信息

Food Chem. 2017 Apr 15;221:891-897. doi: 10.1016/j.foodchem.2016.11.077. Epub 2016 Nov 19.

Abstract

In this work, a highly sensitive quantitative/confirmatory method was developed for the selective determination of marker residue 22,23-dihydroavermectin B in fat, kidney, liver and muscle bovine tissues using UHPLC-MS/MS. A QuEChERS method and a subsequent d-SPE cleaning with MgSO and C18 were used for samples preparation. The method was validated at three levels in each tissue (8.0, 20.0 and 80.0μg/kg for fat, kidney and muscle, 8.0, 16.0 and 40.0μg/kg for liver), taking into account international guidelines. Linearity and matrix effect, accuracy, within-laboratory repeatability, specificity, LOQ, LOD, Q/q relative ion intensities and uncertainty were reported. Recoveries were obtained in the range of 70-120% with within-laboratory repeatability less than 20% for the overall working range. LODs varied from 0.05 to 0.12μg/kg. Compound identification was performed using the relative intensities of monitored transitions. The method could be applied to monitoring withdrawal period specified for ivermectin in cattle.

摘要

在本研究中,开发了一种高灵敏度的定量/确证方法,用于使用超高效液相色谱-串联质谱法(UHPLC-MS/MS)选择性测定牛脂肪、肾脏、肝脏和肌肉组织中的标记残留22,23-二氢阿维菌素B。采用QuEChERS方法以及随后用硫酸镁和C18进行的分散固相萃取(d-SPE)净化处理来制备样品。该方法按照国际指南在每个组织的三个浓度水平(脂肪、肾脏和肌肉为8.0、20.0和80.0μg/kg,肝脏为8.0、16.0和40.0μg/kg)进行了验证。报告了线性和基质效应以及准确度、实验室内重复性、特异性、定量限(LOQ)、检测限(LOD)、Q/q相对离子强度和不确定度。回收率在70%-120%范围内,整个工作范围内实验室内重复性小于20%。检测限在0.05至0.12μg/kg之间。使用监测到的跃迁的相对强度进行化合物鉴定。该方法可用于监测牛中伊维菌素规定的休药期。

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