分散固相萃取-超高效液相色谱-串联质谱法测定农产品中螺虫乙酯及其3种代谢产物残留量
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-C18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~ 100 μg/L质量浓度范围内与其呈良好的线性关系(r2＞0.999), 检出限为0.1 μg/kg, 螺虫乙酯代谢产物S1定量限为1.0 μg/kg, 其余为0.2 μg/kg, 在添加水平为1.0、25、50 μg/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.
标题：分散固相萃取-超高效液相色谱-串联质谱法测定农产品中螺虫乙酯及其3种代谢产物残留量
英文标题：Determination of spirotetramat and its 3 metabolites in agriculture products by ultra performance liquid chromatography-tandem mass spectrometry combined with dispersive solid phase extraction
作者：
张燕 大理州质量技术监督综合检测中心
舒平 大理州质量技术监督综合检测中心
赵浩军 大理州质量技术监督综合检测中心
甘献明 大理州质量技术监督综合检测中心
杨卫花 大理州质量技术监督综合检测中心
杨婷 大理州质量技术监督综合检测中心
李长寿 大理州质量技术监督综合检测中心
中文关键词: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,
英文关键词:dispersed solid phase extraction,agriculture products,spirotetramat and its metabolites,ultra performance liquid chromatography-tandem mass spectrometry,
发表日期：2018-05-09
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