摘要
目的:建立了一种牛乳中氯虫苯甲酰胺、氟苯虫酰胺和2甲4氯的超高效液相色谱-串联质谱(UPLCMS/MS)检测方法。方法:样品经乙腈提取,氯化钠盐析,正己烷除脂,两步低温冷冻离心净化;采用Acquity UPLC BEH C_(18)柱(50 mm×2.1 mm(i.d.),1.7μm)色谱柱分离,以乙腈和0.1%甲酸水溶液为流动相进行梯度洗脱;采用电喷雾电离源,正负离子切换模式扫描,多反应监测模式,以基质标准曲线外标法进行定量。结果:三种农药在10~150 ng/mL范围内线性关系良好(R^(2)>0.999)。分别在5.0、10.0和50.0μg/kg添加水平进行添加回收实验,三种农药的平均回收率在73.3%~117.3%之间,相对标准偏差在1.0%~5.9%之间(n=6);方法的检出限(S/N≥3)和定量限(S/N≥10)分别为1.0、5.0μg/kg。结论:本方法简便、准确、灵敏,适用于牛乳中氯虫苯甲酰胺、氟苯虫酰胺和2甲4氯的同时测定。
Objective:A method was developed for the determination of chlorantraniliprole,flubendiamide and 2-methyl-4-chlorophenoxyacetic acid in milk by ultra performance liquid chromatography-tandemmass spectrometry(UPLC-MS/MS).Methods:The samples were extracted by acetonitrile,salted out by sodium chloride,degreased by n-hexane and purified by two-step cryogenic centrifugation.The analytes were separated by Waters Acquity UPLC BEH C_(18)chromatographic column.The mobile phase was eluted with a gradient of acetonitrile and 0.1%formic acid aqueous solution.The detection was carried out with electrospray ion source,positive and negative ion switching,scanning mode and the quantification was accomplished by external standard method of matrix standard curve.Results:The three pesticides showed a good linear relationship(R2>0.999)in the range of 10~150 ng/mL.With the addition of 5.0,10.0 and 50.0μg/kg in the standard recovery experiment,the recoveries were 73.3%~117.3%and the relative standard deviations were 1.0%~5.9%(n=6).The detection limits(S/N≥3)and the limit of quantification of the method(S/N≥10)were 1.0 and 5.0μg/kg,respectively.Conclusion:This method is simple,accurate and sensitive,which is suitable for simultaneous determination of chlorfenoxamide,fluorofenoxamide and 2-methyl-4-chlorophenoxyacetic acid residues in milk.
作者
文静
莫楠
张立佳
刘丽君
高玉杰
白艳梅
李翠枝
WEN Jing;MO Nan;ZHANG Lijia;LIU Lijun;GAO Yujie;BAI Yanmei;LI Cuizhi(Inner Mongolia Yili Industrial Group Co.,Ltd.,Hohhot 010110,China)
出处
《食品工业科技》
CAS
北大核心
2023年第5期285-291,共7页
Science and Technology of Food Industry
基金
“十三五”国家重点研发计划重点专项(2017YFE0110800)。
关键词
超高效液相色谱-串联质谱
双酰胺类农药
2甲4氯
牛乳
残留
ultra performance liquid chromatography mass spectrometry
bisamide pesticide
2-methyl-4-chlorophenoxyacetic acid
milk
residues
