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建立一种使用液相色谱-串联质谱法对各种动物性食品中18种驱虫药进行多残留定量分析的方法。

Development of an analytical method for multi-residue quantification of 18 anthelmintics in various animal-based food products using liquid chromatography-tandem mass spectrometry.

作者信息

Yoo Kyung-Hee, Park Da-Hee, Abd El-Aty A M, Kim Seong-Kwan, Jung Hae-Ni, Jeong Da-Hye, Cho Hee-Jung, Hacimüftüoğlu Ahmet, Shim Jae-Han, Jeong Ji Hoon, Shin Ho-Chul

机构信息

Department of Veterinary Pharmacology and Toxicology, College of Veterinary Medicine, Konkuk University, Seoul, 143-701, Republic of Korea.

State Key Laboratory of Biobased Material and Green Papermaking, College of Food Science and Engineering, Qilu University of Technology, Shandong Academy of Science, Jinan, 250353, China.

出版信息

J Pharm Anal. 2021 Feb;11(1):68-76. doi: 10.1016/j.jpha.2020.03.008. Epub 2020 Mar 21.

Abstract

In this study, we developed a simple screening procedure for the determination of 18 anthelmintics (including benzimidazoles, macrocyclic lactones, salicylanilides, substituted phenols, tetrahydropyrimidines, and imidazothiazoles) in five animal-derived food matrices (chicken muscle, pork, beef, milk, and egg) using liquid chromatography-tandem mass spectrometry. Analytes were extracted using acetonitrile/1% acetic acid (milk and egg) and acetonitrile/1% acetic acid with 0.5 mL of distilled water (chicken muscle, pork, and beef), and purified using saturated -hexane/acetonitrile. A reversed-phase analytical column and a mobile phase consisting of (A) 10 mM ammonium formate in distilled water and (B) methanol were used to achieve optimal chromatographic separation. Matrix-matched standard calibration curves ( ≥0.9752) were obtained for concentration equivalent to ×1/2, ×1, ×2, ×3, ×4, and ×5 fold the maximum residue limit (MRL) stipulated by the Korean Ministry of Food and Drug Safety. Recoveries of 61.2-118.4%, with relative standard deviations (RSDs) of ≤19.9% (intraday and interday), were obtained for each sample at three spiking concentrations (×1/2, ×1, and ×2 the MRL values). Limits of detection, limits of quantification, and matrix effects were 0.02-5.5 μg/kg, 0.06-10 μg/kg, and -98.8 to 13.9% (at 20 μg/kg), respectively. In five samples of each food matrix (chicken muscle, pork, beef, milk, and egg) purchased from large retailers in Seoul that were tested, none of the target analytes were detected. It has therefore been shown that this protocol is adaptable, accurate, and precise for the quantification of anthelmintic residues in foods of animal origin.

摘要

在本研究中,我们开发了一种简单的筛查程序,用于使用液相色谱 - 串联质谱法测定五种动物源性食品基质(鸡肉、猪肉、牛肉、牛奶和鸡蛋)中的18种驱虫药(包括苯并咪唑类、大环内酯类、水杨酰苯胺类、取代酚类、四氢嘧啶类和咪唑并噻唑类)。分析物使用乙腈/1%乙酸(牛奶和鸡蛋)以及乙腈/1%乙酸与0.5 mL蒸馏水(鸡肉、猪肉和牛肉)进行提取,并使用饱和正己烷/乙腈进行净化。使用反相分析柱和由(A)蒸馏水中的10 mM甲酸铵和(B)甲醇组成的流动相来实现最佳色谱分离。获得了与韩国食品药品安全部规定的最大残留限量(MRL)的×1/2、×1、×2、×3、×4和×5倍浓度相当的基质匹配标准校准曲线(≥0.9752)。在三个加标浓度(MRL值的×1/2、×1和×2)下,每个样品的回收率为61.2 - 118.4%,相对标准偏差(RSD)≤19.9%(日内和日间)。检测限、定量限和基质效应分别为0.02 - 5.5 μg/kg、0.06 - 10 μg/kg和 - 98.8%至13.9%(在20 μg/kg时)。在从首尔的大型零售商购买并测试的每种食品基质(鸡肉、猪肉、牛肉、牛奶和鸡蛋)的五个样品中,未检测到任何目标分析物。因此,已证明该方案适用于动物源性食品中驱虫药残留的定量分析,具有准确性和精密度。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/81bd/7930640/2902bb2878d5/fx1.jpg

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