摘要
目的建立农产品中螺虫乙酯及其3种代谢产物的超高效液相色谱-串联质谱检测方法。方法样品经乙腈涡旋提取,采用乙二胺-N-丙基硅烷(primary secondary amine,PSA)和HC-C_(18)分散固相萃取剂净化,经超高效液相色谱串联质谱仪多反应监测模式检测,外标法定量。结果螺虫乙酯及其3种代谢产物在0.1~100μg/L质量浓度范围内与其呈良好的线性关系(r^2>0.999),检出限为0.1μg/kg,螺虫乙酯代谢产物S1定量限为1.0μg/kg,其余为0.2μg/kg,在添加水平为1.0、25、50μg/kg时,平均回收率为82.5%~99.1%,测定结果的相对标准偏差为1.3%~8.4%(n=6)。结论该方法简单、快速,重复性好,灵敏度和准确度均能满足农产品中螺虫乙酯残留量的测定。
Objective To develop a method for the determination of spirotetramat and its 3 metabolites in agriculture products by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) combined with dispersive solid phase extraction.Methods The samples were extracted with acetonitrile,cleaned up by a mixture of primary secondary amine(PSA) and HC-C18 sorbents,and then detected by UPLC-MS/MS with multiple reaction monitoring mode,and quantified by external standard method.Results Spirotetramat and its 3 metabolites showed good linearities in the range of 0.1-100 μg/L,and the correlation coefficients were more then 0.999.The limits of detection were 0.1 μg/kg for spirotetramat and its 3 metabolites.The limit of quantitative of S1 for metabolite of spirotetramat was 1.0 μg/kg while the rests were 0.2 μg/kg.The average recoveries were in the range of 82.5%-99.1% at the spiked levels of 1.0,25,and 50 μg/kg,and the relative standard deviations(RSDs) were 1.3%-8.4%(n=6).Conclusion The method is simple,rapid,accurate,reproducible,sensitive and accurate,which can be used to determine the residue of spirotetramat in agricultural products.
作者
张燕
舒平
赵浩军
甘献明
杨卫花
杨婷
李长寿
ZHANG Yan;SHU Ping;ZHAO Hao-Jun;GAN Xian-Ming;YANG Wei-Hua;YANG Ting;LI Chang-shou(Dali State Comprehensive Technical lnspection Center, Dali 671000, China)
出处
《食品安全质量检测学报》
CAS
2018年第13期3245-3250,共6页
Journal of Food Safety and Quality
基金
云南省质量技术监督局科技计划项目(2017ynzjkj05)~~
关键词
分散固相萃取
农产品
螺虫乙酯及其代谢产物
超高效液相色谱-串联质谱法
dispersed solid phase extraction
agriculture products
spirotetramat and its metabolites
ultraperformance liquid chromatography-tandem mass spectrometry