China National Food Quality and Safety Supervision and Inspection Center, Haidian District Institute of Products Quality Supervision and Inspection, Beijing, China.
J Agric Food Chem. 2011 Apr 27;59(8):3532-8. doi: 10.1021/jf2006062. Epub 2011 Mar 28.
A reliable, rapid, and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for simultaneous determination of chloramphenicol and aflatoxin M(1) in milk has been developed. This method includes simple extraction of sample with acetonitrile, separation on a MGIII-C(18) column using 5 mM ammonium acetate aqueous solution/methanol (60:40, v/v) as mobile phase, and MS/MS detection using multiple reaction monitoring mode. The method was validated according to Commission Decision 2002/657/EC. The limits of detection (LODs) were 0.05 μg/kg for chloramphenicol and 0.005 μg/kg for aflatoxin M(1.) The limits of quantification (LOQs) were 0.2 μg/kg for chloramphenicol and 0.02 μg/kg for aflatoxin M(1). The recovery values ranged from 88.8% to 100.6%, with relative standard deviation lower than 15% in all cases, when samples were fortified at three different concentrations. The decision limits (CCα) and detection capability (CCβ) of the method were also reported. This method has been successfully applied for simultaneous analysis of chloramphenicol and aflatoxin M(1) residues in milk from local supermarkets in China.
建立了一种可靠、快速、灵敏的液相色谱-串联质谱（LC-MS/MS）方法，用于同时测定牛奶中的氯霉素和黄曲霉毒素 M1。该方法包括用乙腈简单提取样品，在 MGIII-C（18）柱上用 5 mM 乙酸铵水溶液/甲醇（60:40，v/v）作为流动相进行分离，并用多反应监测模式进行 MS/MS 检测。该方法按照委员会决定 2002/657/EC 进行了验证。氯霉素的检测限（LOD）为 0.05 μg/kg，黄曲霉毒素 M1 的检测限（LOD）为 0.005 μg/kg。氯霉素的定量限（LOQ）为 0.2 μg/kg，黄曲霉毒素 M1 的定量限（LOQ）为 0.02 μg/kg。当在三个不同浓度下对样品进行加标时，回收率范围为 88.8%至 100.6%，所有情况下相对标准偏差均低于 15%。该方法的决策限（CCα）和检测能力（CCβ）也得到了报道。该方法已成功应用于中国当地超市牛奶中氯霉素和黄曲霉毒素 M1 残留的同时分析。
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