摘要
采用电子轰击(EI)和负化学(NCI)两种离子源技术建立了气相色谱-质谱联用法(GC-MS)和气相色谱-三重四极杆串联质谱法(GC-MS/MS)测定肉、蛋及内脏中氟虫腈及其代谢物残留的分析方法,并对3种方法进行了比较。样品经乙腈提取,PSA、C18和GCB净化后,由气相色谱-质谱联用EI或NCI技术及GC-MS/MS在多反应离子监测(MRM)模式下进行测定,外标法定量。结果表明,3种方法下氟虫腈及其代谢物在0.001~2.0 mg/L范围内均呈良好的线性关系,相关系数(r2)均大于0.999 0,GC-MS/EI、GC-MS/NCI以及GC-MS/MS/EI的检出限(LOD)分别为0.15、0.05、0.15μg/kg,定量下限(LOQ)分别为0.5、0.2、0.5μg/kg。对电负性强的氟虫腈及其代谢物进行分析,GC-MS/NCI的灵敏度高,在2、50、500μg/kg 3个加标水平下的方法回收率为80.0%~108.0%,相对标准偏差(RSD)为1.1%~7.6%。3种方法可互相补充用于动物源性食品中氟虫腈及其代谢物的检测和确证。
Three analytical methods were established for the determination of fipronil and its metabolite residues in meat,eggs and visceral nitrile by gas chromatography-mass spectrometry （GC-MS ） with electronic ionization （EI ） or negative chemical ionization （NCI ） and gas chromatography-triple quadrupole mass spectrometry （GC-MS/MS ） with EI.And the three methods were compared.The samples were extracted with acetonitrile,and purified with PSA,C 18 and GCB.The extracts were determined by GC-MS combined with EI or NCI techniques and GC-MS/MS with EI in multi-reaction monitoring （MRM ） mode,and quantified by the external standard method.The calibration curves for fipronil and its metabolites were linear in the range of 0.001-2.0 mg/L with correlation coefficients （ r 2 ） higher than 0.999 0.The detection limits （LODs ） of GC-MS/EI,GC-MS/NCI and GC-MS/MS/EI were 0.15,0.05,0.15 μg/kg with the limits of quantitation （LOQs ） of 0.5,0.2,0.5 μg/kg,respectively.The sensitivity of GC-MS method with NCI is much higher than that with EI when analyzing fipronil and its metabolites with several strong electronegative elements in the molecule.The recoveries at three spiked concentration levels of 2,50,500 μg/kg ranged from 80.0 % to 108.0 % with relative standard deviations （RSDs ） of 1.1 % -7.6 % .The three methods could complement each other,and be used in the detection and confirmation of fipronil and its metabolites in animal derived foods.
作者
王艳丽
陈克云
梁秀清
张红霞
胡梅
刘艳明
祝建华
WANG Yan-li;CHEN Ke-yun;LIANG Xiu-qing;ZHANG Hong-xia;HU Mei;LIU Yan-ming;ZHU Jian-hua(Shandong Institute for Food and Drug Control,Jinan 250101,China)
出处
《分析测试学报》
CAS
CSCD
北大核心
2018年第4期440-445,共6页
Journal of Instrumental Analysis
