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Development of an analytical method for multi-residue quantification of 18 anthelmintics in various animal-based food products using liquid chromatography-tandem mass spectrometry
Journal of Pharmaceutical Analysis ( IF 6.1 ) Pub Date : 2020-03-21 , DOI: 10.1016/j.jpha.2020.03.008
Kyung-Hee Yoo , Da-Hee Park , A.M. Abd El-Aty , Seong-Kwan Kim , Hae-Ni Jung , Da-Hye Jeong , Hee-Jung Cho , Ahmet Hacimüftüoğlu , Jae-Han Shim , Ji Hoon Jeong , Ho-Chul Shin

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 n-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 (R2≥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.



中文翻译:

液相色谱-串联质谱法开发多种动物食品中18种驱虫药的多残留定量分析方法

在这项研究中,我们开发了一种简单的筛选程序,用于测定五种动物衍生食品基质(鸡肌肉,猪肉,牛肉,牛奶,和鸡蛋),采用液相色谱-串联质谱分析。使用乙腈/ 1%乙酸(奶和蛋)和乙腈/ 1%乙酸用0.5mL的蒸馏水(鸡肉,猪肉,牛肉和)提取分析物,并且纯化,使用饱和Ñ正己烷/乙腈。使用反相分析柱和由(A)在蒸馏水中的10 mM甲酸铵和(B)甲醇组成的流动相可实现最佳的色谱分离。基质匹配的标准校准曲线(R 2≥0.9752)的浓度相当于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。每个样品在三种加标浓度(MRL值的×1/2,×1和×2)下的回收率达到61.2-118.4%,相对标准偏差(RSD)≤19.9%(日间和日间)。检测限,定量限和基质效应分别为0.02–5.5μg/ kg,0.06–10μg/ kg和-98.8至13.9%(20μg/ kg)。从首尔的大型零售商购买的每种食物基质(鸡肌肉,猪肉,牛肉,牛奶和鸡蛋)的五个样品进行了测试,没有检测到目标分析物。因此,表明该协议是适应性强,准确,

更新日期:2020-03-21
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