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使用液相色谱-串联质谱法测定畜产品中的尼喹酯和丁喹酯。

Determination of nequinate and buquinolate in livestock products using liquid chromatography-tandem mass spectrometry.

作者信息

Nakajima Takayuki, Hayashi Hiroshi, Sasamoto Takeo, Kanda Maki, Kusano Tomoko, Matsushima Youko, Kanai Setsuko, Takeba Kazue, Nagayama Toshihiro

机构信息

Tokyo Metropolitan Institute of Public Health.

出版信息

Shokuhin Eiseigaku Zasshi. 2011;52(3):178-82. doi: 10.3358/shokueishi.52.178.

DOI:10.3358/shokueishi.52.178
PMID:21720123
Abstract

We studied the simultaneous determination of nequinate and buquinolate, which are used as feed additives to prevent coccidiosis, by means of liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS). The sample was extracted with acetonitrile, then loaded onto an HLB mini-column with 20% methanol. After clean-up with 20% methanol, the analytes were eluted with acetonitrile-methanol (1 : 1). The coccidiostats in the purified samples were determined using ESI-MRM mode LC-MS/MS with a sample matrix calibration curve. Mean recoveries of nequinate and buquinolate from 8 kinds of livestocks samples (chicken muscle, chicken liver, chicken heart, swine muscle, swine heart, cattle muscle, sheep muscle, egg) were in the range of 89.5% to 108.6%, and the relative standard deviation values were <20% (n=10) at the levels of 0.01 μg/g and 0.05 μg/g, respectively. The limits of quantification of these compounds were 0.001 μg/g in each sample.

摘要

我们采用液相色谱-串联质谱法(LC-MS/MS)研究了作为饲料添加剂用于预防球虫病的尼喹酯和布喹那酯的同时测定方法。样品用乙腈提取,然后加载到含20%甲醇的HLB小柱上。用20%甲醇净化后,用乙腈-甲醇(1:1)洗脱分析物。使用电喷雾电离-多反应监测模式的LC-MS/MS和样品基质校准曲线测定纯化样品中的抗球虫药。尼喹酯和布喹那酯在8种畜禽样品(鸡肉、鸡肝、鸡心、猪肌肉、猪心、牛肌肉、羊肌肉、鸡蛋)中的平均回收率在89.5%至108.6%之间,在0.01μg/g和0.05μg/g水平下的相对标准偏差值分别<20%(n=10)。这些化合物在每个样品中的定量限均为0.001μg/g。

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