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固相萃取-UPLC-MS/MS法测定牛奶中氟虫腈及其代谢物残留量 预览

Determination of Fipronil and Its Metabolites Residues in Milk by Solid-Phase Extraction-UPLC-MS/MS
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摘要 建立一种固相萃取-超高效液相色谱-串联质谱法同时测定牛奶中氟虫腈及其代谢物(氟甲腈、氟虫腈砜、氟虫腈硫醚)的分析方法。牛奶样品经提取和盐析,Oasis PRiME HLB固相萃取柱通过式净化后,以乙腈-水为流动相,HSS T3色谱柱(2.1mm×100 mm,1.8μm)进行色谱分离,在电喷雾负离子模式下,多反应监测(MRM)方式进行测定,外标法定量。结果表明,氟虫腈及其代谢物在0.05~5.0μg/L浓度范围内均呈良好的线性关系,相关系数r≥0.9976,方法检出限为0.01μg/kg,定量限为0.05μg/kg。在浓度分别为0.5、1、10μg/kg加标水平下,4种化合物的回收率范围为80.6%~101%,相对标准偏差范围为1.0%~6.1%。该方法简单快捷、准确可靠,适用于牛奶中氟虫腈及其代谢物的同时测定。 A method for the simultaneous determination of fipronil and its metabolites(fipronildesulfiny,fipronilsulfone and fipronil sulfide)residues in milk was developed by ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The milk sample was extracted and salted out,and the Oasis PRiME HLB solid phase extraction column was purified by pass-through purification.The acetonitrile-water was used as mobile phase,and the HSS T3 column(2.1 mm×100 mm,1.8μm)was chromatographed in electrospray negative ion mode.Then,the multiple reaction monitoring(MRM)method was used for measurement,and external standard method was used for quantification.The results showed that,the fiproniland its metabolites showed a good linear in the range from 0.05 to 5.0μg/L,and the correlation coefficients r≥0.9976.The limits of detection(LODs)were 0.01μg/kg and the limits of quantification(LOQs)were 0.05μg/kg.At spiked levels of 0.5,1,10μg/kg,the recoveries of the four target analytes were between 80.6%and 101%.The relative standard deviations were between 1.0%and 6.1%.The method was simple and sensitive,and couldbe suitable for the analysis of fipronil and its metabolites residues in milk.
作者 张小刚 王霞 马颖清 丰东升 戴春风 陈美莲 ZHANG Xiao-gang;WANG Xia;MA Ying-qing;FENG Dong-sheng;DAI Chun-feng;CHEN Mei-lian(Shanghai Quality and Safety Testing Centre of Agricultural Product,Ministry of Agriculture-Food Inspection Center,Shanghai 201708,China)
出处 《食品工业科技》 CAS 北大核心 2019年第8期221-224,共4页 Science and Technology of Food Industry
基金 公益性行业(农业)科研专项(201403071).
关键词 氟虫腈 超高效液相色谱-串联质谱 牛奶 固相萃取 fipronil UPLC-MS/MS milk SPE
作者简介 张小刚(1987-),男,硕士,工程师,研究方向:食品、农产品质量与安全,E-mail:zxg6963470@126.com;通讯作者:陈美莲(1963-),女,本科,高级畜牧师,研究方向:农产品质量与安全,E-mail:13601975089@163.com。
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