液相色谱串联质谱法同时测定猪肉中氟雷拉纳和五氯酚残留量  

Simultaneous determination of fluralaner and pentachlorophenol residues in pork by liquid chromatography tandem mass spectrometry

作　　者：伍华雯 刘正才 马欣欣 韩颖 占春瑞 柯秋璇 陈练洪 朱立怡 万建春 WU Huawen;LIU Zhengcai;MA Xinxin;HAN Ying;ZHAN Chunrui;KE Qiuxuan;CHEN Lianhong;ZHU Liyi;WAN Jianchun(Technology Center of Nanchang Customs District,Nanchang 330038,China;Technology Center of Fuzhou Customs District,Fuzhou 350003,China)

机构地区：[1]南昌海关技术中心,南昌330038 [2]福州海关技术中心,福州350003

出　　处：《分析试验室》2024年第5期682-686,共5页Chinese Journal of Analysis Laboratory

基　　金：江西省自然科学基金项目(20212BAB205021)资助。

摘　　要：采用基质分散固相萃取净化结合液相色谱-串联三重四极杆质谱分析技术,基于待测物的油水分配系数和样品前处理正交试验设计,建立了猪肉中氟雷拉纳和五氯酚残留量的检测方法。试样采用酸化乙腈均质提取,提取液加入QuEChERS萃取净化包快速净化,过膜直接上机测定。以5 mmol/L乙酸铵溶液和乙腈为流动相,氟雷拉纳和五氯酚经C18色谱柱梯度洗脱分离后,质谱负离子模式扫描检测。猪肉样品中分别添加1.0, 2.0, 10.0μg/kg 3个浓度水平待测物,氟雷拉纳和五氯酚的加标回收率分别在82.3%~104.0%和71.6%~79.8%之间,相对标准偏差(RSD)分别在3.7%~5.3%和1.2%~3.4%之间。本方法检测氟雷拉纳和五氯酚的定量限均为1.0μg/kg,适用于猪肉中氟雷拉纳和五氯酚残留量的测定。The simultaneous determination of fluralaner and pentachlorophenol residues in pork was developed by using matrix dispersion solid phase extraction to purify the sample solution and liquid chromatography-tandem triple quadrupole tandem mass spectrometry,based on the oil-water distribution coefficient of the tested substance and the orthogonal experimental design of sample pretreatment.After extracting by acidified acetonitrile,the extract was added into the QuEChERS extraction purification package for rapid purification and filtered with the membrane,then the purified liquid was analyzed by LC-MS/MS.With 5 mmol/L ammonium acetate solution and acetonitrile as the mobile phase,fluralaner and pentachlorophenol were separated by gradient elution on the C18 column,and then the negative mode scanning of mass spectrometry was performed.At three spiked concentration levels of 1.0,2.0,10.0μg/kg in the pork,the recoveries of fluralaner and pentachlorophenol were 82.3%-104.0%and 71.6%-79.8%,respectively,and the relative standard deviations(RSDs)were 3.7%-5.3%and 1.2%-3.4%,respectively.The quantitative limits of fluralaner and pentachlorophenol were 1.0μg/kg,which is suitable for the determination of fluralaner and pentachlorophenol residues in pork.

关 键 词：液相色谱串联质谱 猪肉 氟雷拉纳 五氯酚 残留检测 

分 类 号：O657.63[理学—分析化学]