分散固相萃取净化-超高效液相色谱-串联质谱法测定蜂蜜中双甲脒、杀虫脒及其代谢物

Determination of amitraz,chlordimeform,and their metabolites in honey by dispersive solid phase extraction purification-ultra high performance liquid chromatography-tandem mass spectrometry

该研究建立了分散固相萃取-超高效液相色谱-串联质谱(dispersive solid phase extraction-ultra-performance liquid chromatography,UPLC-MS-MS)检测蜂蜜中双甲脒、杀虫脒及其代谢物残留的分析方法。蜂蜜样品2 g加入10 mL水溶液充分混匀,经1%(体积分数)氨化乙腈超声辅助提取后离心,利用N-丙基乙二胺、C18、氨基键合硅胶混合材料进行分散固相萃取净化,采用ACQUITY UPLC BEH C18(2.1 mm×50 mm,1.7μm)色谱柱分离,以甲醇和0.1%(体积分数)甲酸水溶液为流动相进行梯度洗脱,多反应监测模式正离子扫描分析。6种农药及其代谢物平均回收率为84.1%~113.8%,相对标准偏差为0.9%~6.0%,检出限为0.2~0.8μg/kg,定量限为0.7~2.5μg/kg。实验结果表明该方法快速简便、灵敏度高,适用于蜂蜜中双甲脒、杀虫脒及其代谢物残留同时分析。

A method was developed for the determination of amitraz(AMZ),chlordimeform,and their metabolites residues in honey by dispersive solid phase extraction purification-ultra high performance liquid chromatography-tandem.2 g honey sample was fully infiltrated with 10 mL aqueous solution and ultrasonic-assisted extraction with 1%ammonium hydroxide-acetonitrile followed by centrifugation,and then cleaned-up by PSA,C18,and NH 2,the target compounds were analyzed by ACQUITY UPLC BEH C18(2.1 mm×50 mm,1.7μm)column using a mixture of methanol and 0.1%formic acid aqueous solution as mobile phases with gradient elution,the mass spectrometer was operated under MRM mode in positive mode.The average recoveries of 6 pesticides and metabolites were in the range of 84.1%-113.8%,and the relative standard deviation(RSD)was in the range of 0.9%-6.0%,the limit of detection was between 0.2μg/kg and 0.8μg/kg and the limit of quantification was between 0.7μg/kg and 2.5μg/kg for target pesticides,respectively.This method was simple,quick,high sensitivity,and could be used for the routine analysis of amitraz,chlordimeform,and their metabolites residues in honey.