摘要
[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.
作者
陈兴连
林涛
方海仙
李倩
沙凌杰
杨桂仙
李俊
普娅丽
刘宏程
CHEN Xinglian;LIN Tao;FANG Haixian;LI Qian;SHA Lingjie;YANG Guixian;LI Jun;PU Yali;LIU Hongcheng(Quality Standardizing and Testing Technology Institute,Yunnan Academy of Agricultural Sciences,Supervision&Testing Center for Farm Products Quality,Ministry of Agriculture and Rural Affairs(Kunming Section),Kunming 650205,China;Agricultural Products Quality and Safety Inspection Station of Yuan Jiang,Yuxi 653300,Yunnan,China)
出处
《农药》
CAS
CSCD
北大核心
2023年第9期657-663,共7页
Agrochemicals
基金
农产品绿色生产及质量安全控制关键技术研究与示范应用(重大科技专项)(202002AE320005)
云南省庞国芳院士工作站(202305AF150015)
特色农产品质量安全检测关键技术研究与应用(202102AE090021)。