液相色谱-三重四级杆质谱法测定苹果中 腈苯唑农药残留
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。
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.
标题：液相色谱-三重四级杆质谱法测定苹果中 腈苯唑农药残留
英文标题：Analysis of fenbuconazole residue in apple using ultra pressure liquid chromatography-triple quadrupole mass spectrometry
作者：
刘春华 中国热带农业科学院分析测试中心,海南省热带果蔬产品质量安全重点实验室
张群 中国热带农业科学院分析测试中心,海南省热带果蔬产品质量安全重点实验室
阳辛凤 中国热带农业科学院分析测试中心,海南省热带果蔬产品质量安全重点实验室
乐渊 中国热带农业科学院分析测试中心,海南省热带果蔬产品质量安全重点实验室
吴南村 中国热带农业科学院分析测试中心,海南省热带果蔬产品质量安全重点实验室
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,
发表日期：2014-08-28
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