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首页> 外文期刊>Food Control >Development and validation of a method for the determination of sulfonamides in animal feed by modified QuEChERS and LC-MS/MS analysis.
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Development and validation of a method for the determination of sulfonamides in animal feed by modified QuEChERS and LC-MS/MS analysis.

机译：改进的QuEChERS和LC-MS / MS分析方法用于动物饲料中磺酰胺测定方法的开发和验证。

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摘要

A multiresidue method for the quantification of 13 sulfonamides in animal feed is described. It involves the application of a modified QuEChERS procedure followed by HPLC-MS/MS (high performance liquid chromatography coupled to tandem mass spectrometry) analysis. The best conditions for the extraction solution and PSA (primary secondary amine) mass were determined. After optimization, the method was validated according to the European Commission Decision 2002/657/EC. The validation levels employed were 25, 50 and 75 mug kg--1. Acceptable values were obtained for the following parameters: linearity (0.9864 < r2 < 0.9993), decision limit (50.4 mug kg--1 < CC alpha < 55.8 mug kg--1), detection capability (50.7 mug kg--1 beta < 55.8 mug kg--1), limit of quantification (0.9 mug kg--1 < LOQ < 7.1 mug kg--1), accuracy (86.0 < recovery rates < 106.8), precision [(3.6 < repeatability < 19.5), (5.5 < intermediate precision < 21.6)], measurement uncertainty (MU) (4.1 < MU < 32.6) and selectivity. These findings met the Codex requirements, which allow for the routine use of the method by the laboratories linked to the Ministry of Agriculture, Livestock and Food Supply of Brazil. Finally, the method was applied to real samples and only one of them showed positive for sulfamethazine, however, with a concentration below the LOQ of the method
机译：描述了一种定量动物饲料中13种磺酰胺的多残留方法。它涉及应用改良的QuEChERS程序，然后进行HPLC-MS / MS（高效液相色谱与串联质谱联用）分析。确定了萃取溶液和PSA（伯仲胺）质量的最佳条件。优化后，该方法已根据欧洲委员会第2002/657 / EC号决定进行了验证。使用的验证水平为25、50和75马克杯kg -1 。获得以下参数的可接受值：线性（0.9864 i> r 2 <0.9993），决策极限（50.4马克杯kg -1 < CC alpha <55.8杯子kg -1 ），检测能力（50.7杯子kg -1 beta <55.8千克kg -1 ），定量限（0.9千克kg -1 ），精度（86.0 <回收率<106.8），精度[（3.6 <重复性<19.5），（5.5 <中等精度<21.6）]，测量不确定度（MU）（4.1​​

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