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目的建立苹果中杀铃脲的超高效液相色谱-串联质谱(UPLC-MS/MS)快速测定方法。方法苹果样品通过乙腈匀浆提取,用固相萃取小柱净化,甲醇-二氯甲烷(1:19,v:v)淋洗、洗脱后,选用C18(100 mm×2.1 mm i.d.,1.7μm)作为分析柱,甲醇/1 mmol/L乙酸铵梯度洗脱,经高效液相色谱分离,在多反应监测模式(MRM)及电喷电离方式(ESI+)下串联质谱法进行测定,基质配标准曲线定量。结果分析物在0.01~0.50 mg/L范围内有良好的线性关系,相关系数r>0.99,空白样品中分析物在添加水平为0.01、0.02、0.05 mg/kg时,平均回收率在80.0%~84.8%之间,相对标准偏差为4.9%~8.8%,定量限为0.005 mg/kg。结论本方法简单快速、灵敏度高、准确度好,能满足定量分析的要求。
Objective To establish an HPLC-MS / MS method for rapid determination of triflumuron in apple. Methods The apple samples were extracted by acetonitrile homogenate and eluted with solid-phase extraction cartridge and eluted with methanol-dichloromethane (1:19, v: v) ) As analytical column, gradient elution with methanol / 1 mmol / L ammonium acetate, high performance liquid chromatography and tandem mass spectrometry in multiple reaction monitoring mode (MRM) and electrospray ionization mode (ESI +), Curve quantitative. Results The analyte had a good linear relationship in the range of 0.01-0.50 mg / L with the correlation coefficient r> 0.99. The average recoveries of the analytes in the blank samples were 0.01%, 0.02%, 0.05 mg / kg, 84.8%, the relative standard deviation was 4.9% ~ 8.8%, and the limit of quantification was 0.005 mg / kg. Conclusion The method is simple and fast, high sensitivity and accuracy, and can meet the requirements of quantitative analysis.