超高效液相色谱-串联质谱法测定动物源性食品中硝基呋喃代谢物
目的 建立动物源性食品中四种硝基呋喃代谢物的超高效液相色谱串联质谱(ultra pressure liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)的快速检测方法。方法 样品经盐酸溶液水解, 邻硝基苯甲醛(2-NBA) 37 ℃衍生16 h后, 调节衍生液的pH =7.6, 用乙酸乙酯提取。分析物采用电喷雾电离, 正离子扫描, 多反应检测模式(MRM), 基质匹配内标标准曲线法定量。结果 四种代谢物的工作曲线在0.1?10.0 ?g/L浓度范围内线性良好, 相关系数R2均达到了0.995以上, 氨基脲(SEM或SCA) 与1-氨基-乙内酰脲(AHD)最低检出限均为0.1 μg/kg, 5-吗啉甲基-3-氨基-2-恶唑烷基酮(AMOZ)与3-氨基-2-恶唑烷基酮(AOZ)最低检出限均为0.05 μg/kg。平均回收率在91.8%?107.0%之间, 相对标准偏差均小于10%。结论 样品前处理简单、测定时间短、灵敏度高, 适用于猪肉、牛肉、鸡肉、猪肝和水产品(鱼类及虾类)中硝基呋喃类代谢物残留的快速测定。
Objective A rapid analytical method for the detection of metabolites of nitrofuran in food by the ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was established. Methods The metabolites in food samples were released in HCl solution, and derived using 2-nitrobenzaldehyde (2-NBA) at 37 ℃ for 16 h. The pH values of derivates were adjusted to 7.6, and then the analytes were extracted by ethyl acetate. Identification was achieved by electrospray ionization in positive mode (ESI ) using multiple reaction monitoring (MRM). The quantification was performed by the matrix matched internal standards. Results The calibration curves of the four analytes showed a good linearity in the concentrations of 0.1?10 μg/L with R2 above 0.995. The limits of detection of SCA and AHD were 0.1 μg/kg, and the limits of detection of AMOZ and AOZ were 0.05 μg/kg. Recoveries were between 91.8% and 107.0% with the relative standard deviations (RSD) less than 10%. Conclusion This method simplifies the sample pre-treatment, and reduces the detection time, and it is a fast, highly selective and sensitive assay. The method can apply to the rapid detection of nitrofuran metabolites in pork, beef, chicken, porcine liver, fish and shrimp.
标题：超高效液相色谱-串联质谱法测定动物源性食品中硝基呋喃代谢物
英文标题：Determination of metabolites of nitrofuran in food samples by ultra perform-ance liquid chromatography-tandem mass spectrometry
作者：
刘柏林 安徽省疾病预防控制中心
谢继安 安徽省疾病预防控制中心
赵紫微 安徽省疾病预防控制中心
韦莹 安徽省疾病预防控制中心
单晓梅 安徽省疾病预防控制中心
中文关键词:超高效液相色谱-串联质谱法,硝基呋喃代谢物,动物源性食品,测定,
英文关键词:ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS),nitrofuran metabolites,animal tissues food,determination,
发表日期：2013-11-11
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