苹果中杀铃脲残留量的快速测定方法研究

Methodology for rapid determination of triflumuron residue in apple

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 An ultra performance liquid chromatography-tandem mass spectrometry analysis (UPLC-MS/MS) was established for the determination of the residues of triflumuron pesticide in apple. Me-thods The samples were extracted by ultrasonic extraction with acetonitrile and cleaned with solid-phase ex-traction. The separation was performed on a C18 column(100 mm×2.1 mm i.d., 1.7 μm), the gradient mobile phase consisting of 1 mmol /L ammonium acetate and methanol. The separation was achieved by UPLC, and then the identification and quantification were performed using MS/MS with multiple-reaction monitoring (MRM) and positive electrospray ionization (ESI+) 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 80.0%~84.8%at the spiked levels of 0.01, 0.02 mg/kg and 0.05 mg/kg with relative standard deviations (RSDs) of 4.9%~8.8%. Conclusion The method is sensitive and accuracy and it is suitable for quantitative determi-nation of triflumuron pesticides in apple.