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。结论本方法灵敏度高、准确度好,能满足定量分析的要求。
Objective An ultra performance liquid chromatography tandem mass spectrome-try(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 de-tected 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 correla-tion coefficient over 0.99. The limits of quantitation (LOQ) for the pesticide residue were 0.005 mg/kg. The aver-age 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.
出处
《食品安全质量检测学报》
CAS
2014年第2期428-434,共7页
Journal of Food Safety and Quality
