液相色谱-三重四级杆质谱法测定苹果中 腈苯唑农药残留

Analysis of fenbuconazole residue in apple using ultra pressure liquid chromatography-triple quadrupole mass spectrometry

中文关键词:  苹果  腈苯唑  液相色谱-三重四级杆质谱(UPLC-QQQ-MS/MS)

英文关键词:apple  fenbuconazole  ultra pressure liquid chromatography-triple quadrupole mass spectrometry

中文摘要:

      目的 为加强我国苹果中腈苯唑农药残留的监控, 保护我国苹果在国际贸易中的合理地位, 建立了苹果中腈苯唑的液相色谱-三重四级杆质谱(UPLC-MS/MS)测定方法。方法 样品经乙腈提取, 超高效液相色谱-串联质谱下进行测定。结果 目标物在0.005~0.50 mg/L范围内成线性, 相关系数r>0.99, 空白样品中分析物在添加浓度为0.01、0.02、0.05 mg/kg时, 平均回收率为89.6%~93.0%, 相对标准偏差为2.4%~7.9%, 定量限为0.01 mg/kg。结论 本方法操作简便、灵敏度高、准确度好, 能满足农残检测分析的要求。

英文摘要:

      Objective To establish the simultaneous determination method for the residues of fenbuconazole pesticide in apple by ultra pressure liquid chromatography-triple quadrupole mass spectrometry (UPLC-QQQ-MS/MS). Methods The samples were extracted by ultrasonic extraction with acetonitrile. The analysis was detected by UPLC-MS/MS under positive electrospray ionization (ESI+) and multiple reaction monitoring (MRM) mode. The matrix-matched external standard calibration curves were used for the quantitative analysis. Results Under the optimum conditions, the method showed a good linearity in the range of 0.005~0.50 mg/L with correlation coefficient over 0.99. The limit of quantitation (LOQ) for the pesticide residue was 0.01 mg/kg. The average recoveries of pesticides residues were 89.6%~93.0% at the spiked levels of 0.01, 0.02 and 0.05 mg/kg with relative standard deviations (RSDs) of 2.4%~7.9%. Conclusion The method is sensitive and accurate, and it is suitable for simultaneous quantitative determination of fenbuconazole pesticides in apple.