快速滤过型净化结合超高效液相色谱-串联质谱法测定姬松茸中农药残留

Determination of pesticide residues in Agaricus blazei Murill by multi-plug filtration cleanup method combined with high performance liquid chromatography-tandem mass spectrometry

[目的]建立快速滤过型净化-超高效液相色谱-串联质谱测定姬松茸中残留农药的方法。[方法]姬松茸样品加水浸润后农药经乙腈提取,乙腈和水通过盐析分层,取上层乙腈经无水硫酸镁、PSA、C18、Florisil净化材料装填的m-PFC柱净化,目标物经ACQUITY UPLC BEH C18色谱柱分离,正离子多反应监测模式采集,外标法定量。[结果]在0.00015~0.2、0.2~0.6 mg/L线性范围内,5种农药线性关系良好,线性相关系数大于0.99,检出限为0.0002~0.0005 mg/kg,定量限为0.0006~0.0015 mg/kg。在1倍(低)、10倍(中)、50倍(高)定量限浓度下的添加回收率为89.5%~105.6%,相对标准偏差为3.4%~9.1%。[结论]该方法提取效率高,净化效果好,有效提高了姬松茸中农药测定值的准确性,同时为姬松茸日常质量安全监测提供了技术保障。

[Aims]To establish a method for the determination of pesticide residues in Agaricus blazei Murill by multi-plug filtration cleanup(m-PFC)-ultra high performance liquid chromatography tandem mass spectrometry(UPLC-MS).[Methods]After the Agaricus blazei murill sample was soaked in water,the pesticides were extracted by acetonitrile,the acetonitrile and water were separated by salting-out,and the upper acetonitrile was purified by m-PFC column packed with anhydrous magnesium sulfate,PSA,C18 and Florisil.The targets were separated by ACQUITY UPLC BEH C18 column,gathered by positive ion multi-reaction monitoring mode,quantified by external standard method.[Results]The results showed that the linear relationship of the five pesticides was good in the linear range of 0.00015-0.2 and 0.2-0.6 mg/L,the linear correlation coefficient was more than 0.99,the detection limit was 0.0002-0.0005 mg/kg,and the limit of quantification(LOQ)was 0.0006-0.0015 mg/kg.The recoveries were 89.5%-105.6%at 1(low),10(medium)and 50(high)times the LOQ and the relative standard deviations were 3.4%-9.1%.[Conclusions]This method,having high extraction efficiency and good purification effect,can effectively improve the accuracy of pesticide determination in A.blazei murill,and provides a technical support for daily quality and safety monitoring in A.blazei at the same time.