超高效液相色谱-串联质谱法同时测定梨中22种农药残留

Simultaneous determination of 22 kinds of pesticide residues in pear by ultra-high performance liquid chromatography-tandem mass spectrometry

目的建立一种超高效液相色谱-串联质谱法测定梨中苯酰菌胺、吡蚜酮、氟虫脲等22种农药残留的分析方法。方法样品经过高速匀浆后加入乙腈进行提取,采用ReproSil 100 C_(18)柱(150 mm×2.1 mm, 5μm),流速为0.3mL/min,柱温为35℃进行分离,应用超高效液相色谱-串联质谱正离子模式下的多反应监测(multiple reaction monitoring, MRM)扫描进行定性定量分析。结果在浓度测定范围0.010～0.20 mg/L内, 22种农药均成线性关系,相关系数(r^2)为0.9709～0.9998。在0.010、0.050、0.10 mg/kg 3个添加水平下, 22种化合物的回收率为71.4%～106.7%,相对标准偏差为0.7%～9.9%;检出限为0.90～4.6μg/kg,方法定量限3.0～15.4μg/kg。在实际梨样品检测到5种农药残留。结论此方法简便快速、准确度高,可用于梨样品中22种农药残留的测定。

Objective To develop an analytical method based on ultra-high performance liquid chromatographytandem mass spectrometry(UPLC-MS/MS)to analyze 22 kinds of pesticide residues of zoxamide,pymetrozin,flufenoxuro and so on.Methods The samples were homogenized at high speed and extracted with acetonitrile,and separated by ReproSil 100 C18(150 mm×2.1 mm,5μm)chromatographic column,with the flow rate of 0.3 mL/min and column temperature of 35℃,and were quantified by ultra-high performance liquid chromatography-tandem mass spectrometry in a positive ion multiple reaction mode.Results The result showed that excellent linear relationships for 22 pesticides were observed in the concentration range of 0.01-0.2 mg/L with the regression coefficients of 0.9709-0.9998.Under the 3 spiked levels of 0.010,0.050 and 0.10 mg/kg,the average recovery rates of 22 pesticides were in the range of 71.4%-106.7%,with relative standard deviations of 0.7%-9.9%.The limits of detection and limits of quantitation were 0.90-4.6μg/kg and 3.0-15.4μg/kg,respectively.Totally 5 pesticide residues were detected in pear samples.Conclusion The method is simple,rapid and accurate,which can be used for the determination of 22 pesticide residues in pear samples.