Desmarchelier Aurélien, Anizan Sébastien, Minh Tien Mai, Savoy Marie-Claude, Bion Cindy
a Nestlé Research Center , Institute of Food Safety and Analytical Science , Lausanne , Switzerland.
b Nestlé Quality Assurance Center , Cergy , France.
Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2018 Apr;35(4):686-694. doi: 10.1080/19440049.2018.1427894. Epub 2018 Feb 20.
An LC-MS/MS method is presented for screening five tetracyclines and their epimers in a broad range of food products. The scope of matrices includes meat-, fish-, seafood-based products, various dairy ingredients, infant formulae and fats. The method principle is based on a liquid-liquid extraction with aqueous ethylenediaminetetraacetic acid (EDTA) and acetonitrile followed by a freezing step to promote phase separation at low temperature. After defatting with hexane, sample extracts were evaporated and reconstituted before injection onto the LC-MS/MS system. The addition of oxalic acid in the aqueous mobile phase was mandatory to maintain good peak shape and sensitivity over the run. The screening is based upon a double preparation of each sample, one 'as such' and a second one with the analytes spiked in the sample, in order to mitigate the risk of false negative response. The method was validated according to the European Community Reference Laboratories Residues Guidelines. A total of 93 samples were included in the validation by two independent laboratories giving both false-negative and false-positive rates at 0% for all compounds. Over the last two years, 2600 samples were analysed routinely and only one chicken sample was found above the regulatory limit.
本文介绍了一种液相色谱-串联质谱法，用于在多种食品中筛查五种四环素及其差向异构体。基质范围包括肉类、鱼类、海鲜类产品、各种乳制品成分、婴儿配方奶粉和脂肪。该方法的原理是基于用乙二胺四乙酸（EDTA）水溶液和乙腈进行液液萃取，随后进行冷冻步骤以促进低温下的相分离。用己烷脱脂后，将样品提取物蒸发并复溶，然后注入液相色谱-串联质谱系统。在流动相水溶液中添加草酸是必要的，以在整个运行过程中保持良好的峰形和灵敏度。筛查基于对每个样品进行双重制备，一个是“原样”，另一个是在样品中添加分析物，以降低假阴性响应的风险。该方法根据欧洲共同体参考实验室残留指南进行了验证。两个独立实验室共纳入93个样品进行验证，所有化合物的假阴性率和假阳性率均为0%。在过去两年中，对2600个样品进行了常规分析，仅发现一个鸡肉样品超过监管限量。
