QuEChERS结合高效液相色谱-串联质谱法同时测定山楂中螺虫乙酯及其4种代谢物残留

Simultaneous determination of spirotetramat and its 4 kinds of metabolites residues in Crataegus pinnatifida Bunge. by QuEChERS combined with high performance liquid chromatography-tandem mass spectrometry

中文关键词:  螺虫乙酯  代谢物  山楂  QuEChERS  高效液相色谱-串联质谱法

英文关键词:spirotetramat  metabolites  Crataegus pinnatifida Bunge.  QuEChERS  high performance liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立QuEChERS结合高效液相色谱-串联质谱法(high performance liquid chromatography -tandem mass spectrometry, HPLC-MS/MS)同时测定山楂(Crataegus pinnatifida Bunge.)中螺虫乙酯及其4种代谢物残留的分析方法。方法 采用QuEChERS前处理方法, 样品经过1%乙酸-乙腈涡旋振荡提取及氯化钠盐析作用后, 使用石墨化碳黑(graphitized carbon black, GCB)和N-丙基乙二胺(primary secondary amine, PSA)净化, 经色谱柱分离, 0.1%甲酸水溶液-乙腈流动相梯度洗脱。多重反应监测模式下, 高效液相色谱-串联质谱法测定, 基质匹配标准溶液的外标法定量。结果 螺虫乙酯及其代谢产物在0.005~0.500 mg/L范围内呈良好的线性关系, 相关系数r2大于0.98, 最低检测浓度为0.01 mg/kg。当添加水平为0.01、0.10、1.00 mg/kg时, 山楂中螺虫乙酯及其代谢产物的平均回收率为83%~106%, 相对标准偏差(relative standard deviations, RSDs)为0.6%~11.0%。结论 该方法操作简单快捷、反应灵敏、重现性好, 符合NY/T 788—2018《农作物中农药残留试验准则》的要求, 适用于测定山楂中螺虫乙酯及其代谢产物残留。

英文摘要:

      Objective To establish a method for the simultaneous determination of spirotetramat and its 4 kinds of metabolites residues in Crataegus pinnatifida Bunge. by QuEChERS combined with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Method QuEChERS method was adopted, and after the sample was extracted with 1% acetic acid-acetonitrile vortex oscillation and salted out with sodium chloride, purified with graphitized carbon black (GCB) and primary secondary amine (PSA), separated by a chromatographic column with gradient elution of 0.1% formic acid aqueous solution-acetonitrile as mobile phase. Under multiple response monitoring mode, it was determined by HPLC-MS/MS, and quantified by the external standard method of matrix matching standard solution. Results The spirotetramat and its metabolites showed good linear relationship in the range of 0.005?0.500 mg/L, the correlation coefficients (r2) were more than 0.98, and the minimum detection concentration was 0.01 mg/kg. When the addition levels were 0.01, 0.10, 1.00 mg/kg, the average recoveries of spirotetramat and its metabolites in Crataegus pinnatifida Bunge. were 83%?106%, and the relative standard deviations (RSDs) were 0.6%?11.0%. Conclusion This method is simple and rapid, sensitive and reproducible, which meets the requirements of NY/T 788—2018 Test guidelines for pesticide residues in crops, and is suitable for the determination of spirotetramat and its metabolite residues in Crataegus pinnatifida Bunge.