超高效液相色谱-串联质谱法测定苹果中刺糖菌素A

Determination of spinosyn A residues in apple by ultra pressure liquid chromatography-tandem mass spectrometry

中文关键词:  苹果  刺糖菌素A  超高压液相色谱-串联质谱(UPLC-MS/MS)

英文关键词:apple  spinosyn A  ultra performance liquid chromatography tandem mass spectrometry

中文摘要:

      目的 建立苹果中刺糖菌素A的超高效液相色谱-串联质谱(UPLC-MS/MS)测定方法。方法 样品通过乙腈匀浆提取, 在电喷电离方式(ESI )、多反应监测模式(MRM)下进行测定, 基质配标准曲线定量。结果 分析物在0.005~0.50 mg/kg范围内成线性, 相关系数r>0.99, 空白样品中分析物在0.01、0.02、0.10 mg/kg三个不同添加水平时, 平均回收率在93.3%~101.7%之间, 相对标准偏差为5.2%~7.4%, 定量限为0.005 mg/kg。

英文摘要:

      Objective An ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS) was established for the simultaneous determination the residues of spinosyn A pesticide in apple. 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 limits of quantitation (LOQ) for the pesticide residue were 0.005 mg/kg. The average recoveries of pesticides residues were 93.3%~101.7% at the spiked levels of 0.01, 0.02 mg/kg and 0.10 mg/kg with relative standard deviation (RSDs) of 5.2%~7.4%. Conclusion The method is sensitive and accurate and it is suitable for simultaneous quantitative determination of spinosyn A pesticides in apple.