固相萃取-同位素稀释超高效液相色谱-串联质谱法测定动物源性食品中24种β2-受体激动剂

Simultaneous determination of 24 β2-agonists in animal derived food by solid phase extraction isotopes-dilution technique and ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  β2-受体激动剂  超高效液相色谱串联质谱  动物源性食品

英文关键词:β2-agonists  ultra performance liquid chromatography tandem mass spectrometry  animal derived food

中文摘要:

      目的 建立固相萃取-同位素稀释超高效液相色谱/串联质谱法同时测定动物源性食品中24种β2-受体激动剂残留量的检测方法。方法 样品经β-葡萄糖苷酸酶水解, 过混合阳离子(MCX)固相萃取柱净化。采用乙腈和含有0.1%甲酸的水为流动相, 梯度洗脱, 质谱(ESI+)采用多离子检测模式(MRM)对24种β2-受体激动剂残留量进行检测。结果 该方法各组分的最低定量限为0.1~0.5 μg/kg, 在0.1~20.0 μg/kg浓度下呈现良好的线性关系, 加标回收率为72.5%~109.3%。结论 该方法操作简便, 准确, 快速, 灵敏, 可同时检测24种β2-受体激动剂的残留量。

英文摘要:

      Objective To establish a novel method for simultaneous determination of 24 kinds of β2-agonists in animal derived food by solid phase extraction-isotopes dilution technique and ultra performance liquid chromatography combined with tandem mass spectrometry. Methods Samples were enzymolysised with β-glucuronidase enzyme. The chromatographic concentration and purification were performed with MCX, and the β2-agonists in the extracts were separated on a reversed phase using a gradient elution program of containing 0.1% formic acid as mobile phase. Using mass spectrometry (ESI+) with multiple reactions monitoring (MRM), identification of the major components of 24 kinds of β2-agonists residues was per-formed. Results This method showed a good linearity in the range of 0.1~20.0 μg/kg for 24 kinds of β2-agonists in animal derived food, the limits of quantitation (LOQ) of this method were 0.1~0.5 μg/kg, and relative standard deviations (RSDs) were 72.5%~109.3%. Conclusion The method is simple, accurate, fast, and sensitive, which is suitable for detecting 24 kinds of β2-agonist residues in animal derived food.