建立了QuEChERS-超高效液相色谱-串联质谱法快速测定动物源性食品中矮壮素残留的分析方法。样品经乙腈提取,无水硫酸镁、C18及N-丙基乙二胺吸附剂净化,采用Venusil MP C18(2)色谱柱分离,内标法定量。结果表明,矮壮素在0.05 ~200 μg/L线性良好,相关系数(R2)为0.999 9,方法的定量限为0.2~0.5 μg/kg;以猪肉、牛肉、羊肉、鸡肉、猪肝、牛肝、羊肝、鸡肝、鸡蛋和奶粉为基质,矮壮素在1.0、20.0和500.0 μg/kg 3个水平下的加标回收率为84%~103%,相对标准偏差为2.13%~6.49%;对市售的271份动物源性样品进行检测,检出阳性样品26份,含量范围为1.06~14.5 μg/kg。该方法简便、高效、快速、准确、灵敏度高,适用于动物源性食品中矮壮素残留的快速定量检测。
A rapid method for the determination of chlormequat (CCC) residues in animal-derived food by QuEChERS-UPLC-MS/MS was established. The samples were extracted with acetonitrile and purified with anhydrous magnesium sulfate, C18 and PSA adsorbents. The analytes were separated on a Venusil MP C18(2) column, then quantitative analysis by internal standard method. The calibration curve showed good linearity in the range of 0.05-200 μg/L for CCC, with correlation coefficients (R2) of 0.999 9. The limits of quantification (LOQ) of the method were 0.2-0.5 μg/kg. The recoveries of CCC in the pork, beef, mutton, chicken, pig liver, beef liver, sheep liver, chicken liver, egg and milk powder matrices at the spiked levels of 1.0, 20.0 and 500.0 μg/kg were 84%-103%, and the relative standard deviations were 2.13%-6.49%. The method was used to detect 271 animal origin samples in which 26 positive samples were detected and the contents ranged from 1.06 to 14.5 μg/kg. The method is a simple, efficient, rapid, accurate and high sensitivity, and it is suitable for the rapid quantitative detection of CCC residues in animal-derived food.
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