QuEChERS-超高效液相色谱-串联质谱法同时测定生姜中多种农药及代谢物残留  

Determination of multiple pesticide and metabolite residues in ginger by QuEChERS-liquid chromatography-tandem mass spectrometry

作　　者：张金环[1] 程艳宇[1] 李桂红 李伟霞 朱欢 ZHANG Jinhuan;CHENG Yanyu;LI Guihong;LI Weixia;ZHU Huan(Tianjin Dairy and Food Monitoring Center Limited Company,Tianjin 300392,China)

机构地区：[1]天津市乳品食品监测中心有限公司,天津300392

出　　处：《世界农药》2023年第5期31-37,共7页World Pesticide

摘　　要：为建立生姜中农药残留快速同时检测方法,通过优化QuEChERS前处理方法并结合超高效液相色谱-三重四极杆串联质谱(UPLC-MS/MS)技术,用乙腈提取样品,氯化钠(NaCl)为脱水剂,经丙基乙二胺(PSA)和GCB混合净化剂净化,WatersACQUITYUPLC BEHC18色谱柱(2.1mm×100 mm,1.7μm)分离,超高效液相色谱-串联质谱测定。考察了MgSO4、PSA、GCB用量对农药及代谢物添加回收率的影响。结果表明:2 mL提取上清液中加入300 mg无水MgSO4、50 mg PSA和5.0 mg GCB时净化效果最好。在3个添加水平下,38种农药及6种代谢物在生姜中的回收率为71.9%~102.2%,相对标准偏差(RSD)为1.1%~8.9%。方法的检出限为1.0~5.0μg/kg。该方法简便、快速、可靠,可用于日常工作快速筛查、确证生姜中农药残留,具有一定推广应用价值。A rapid detection method of multipesticide residues in ginger was established by optimizing QuEChERS pretreatment method combined with ultra high performance liquid chromatochromatosure-triple quadrupole tandem mass spectrometry(UPLC-MS/MS).The samples were extracted by acetonitrile and purified by propyl ethylenediamine(PSA)and graphitized carbon black(GCB)mixture using sodium chloride(NaCl)as dehydrating agent.The samples were separated on Waters ACQUITY UPLC BEH C18 column(2.1 mm×100 mm,1.7μm)and determined by UPLC-MS/MS.The effects of the dosage of MgSO4,PSA,and GCB on the recovery rate of pesticide and metabolite addition were investigated in detail.The results showed that the purification effect was the best when 300 mg anhydrous magnesium sulfate,50 mg PSA and 5.0mg GCB were added into 2 mL supernatant.The recoveries of 38 pesticides and 6 metabolites were 71.9%-102.2%,and the relative standard deviations(RSD)were 1.1%-8.9%.The detection limit was 1.0-5.0μg/kg.The method is simple,rapid and reliable,and can be used in the daily work of rapid screening and confirmation of many pesticide residues in ginger,and has certain popularization value.

关 键 词：QUECHERS 超高效液相色谱-串联质谱 农药残留 生姜 

分 类 号：TQ450.2[化学工程—农药化工]