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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。结论本方法灵敏度高、准确度好,能满足定量分析的要求。
Objective To establish a method for the determination of spinosyn A in apple by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS / MS). Methods The samples were extracted by acetonitrile homogenization and determined by electrospray ionization (ESI +) and multiple reaction monitoring (MRM). The matrix was quantified with a standard curve. Results The analytes were linear in the range of 0.005-0.50 mg / kg with a correlation coefficient r> 0.99. The average recoveries of the analytes in the blank samples were 93.3% -101.7 at three different levels of 0.01, 0.02 and 0.10 mg / kg %, The relative standard deviation was 5.2% ~ 7.4%, the limit of quantification was 0.005 mg / kg. Conclusion The method has high sensitivity and accuracy, and can meet the requirements of quantitative analysis.