气相色谱-三重四极杆-串联质谱法测定莲子中59种农药残留

Determination of 59 kinds of pesticide residues in lotus seeds by gas chromatography-triple quadrupole-tandem mass spectrometry

中文关键词:  莲子  农药残留  气相色谱-三重四极杆-串联质谱法

英文关键词:lotus seeds  pesticide residues  gas chromatography-triple quadrupole tandem mass spectrometry

中文摘要:

      目的 建立气相色谱-三重四极杆-串联质谱法(gas chromatography-triple quadrupole-tandem mass spectrometry, GC-MS/MS)测定莲子中59种农药残留量的快速检测方法。方法 利用乙腈提取样品, 分散固相萃取法净化样品, 采用HP-5ms毛细管色谱柱(30 m×320 μm, 0.25 μm)分离, 高纯氦作为载气, 流速1.0 mL/min, 不分流进样, 进样器温度280 ℃, 传输线温度300 ℃, 质谱检测器温度280 ℃, GC-MS/MS检测采用选择多反应监测模式(multiple reaction monitoring, MRM)定量分析。结果 59种农药在50~1500 ng/mL范围内呈现良好的线性关系, 相关系数(r2)大于0.99, 各农药定量限(S/N=10)为0.0005~0.02 mg/kg, 3个浓度添加水平上的加标回收率范围均为62.3%~115.0%, 相对标准偏差(relative standard deviation, RSD) (n=6)范围为0.76%~15.33%。结论 该方法灵敏度高, 准确性好, 快速简便, 适用于莲子中59种农药残留量的快速测定和验证。

英文摘要:

      Objective To establish a rapid method for the determination of 59 kinds of pesticide residues in lotus seeds by gas chromatography-triple quadrupole-tandem mass spectrometry (GC-MS/MS). Methods The samples were extracted by acetonitrile, cleaned up with dispersive solid phase extraction method. Then separated by HP-5ms capillary column (30 m×320 μm, 0.25 μm). High purity helium was used as the carrier gas at a flow rate of 1.0 mL/min, with no split flow into the sample. Injector temperature was 280 °C, transmission line temperature was 300 °C, mass spectrometer detector at 280 °C, and samples was detected by gas chromatography-triple quadrupole-tandem mass spectrometry with multiple reaction monitoring (MRM) mode for quantification. Results The linearities were good for the 59 kinds of pesticides in the range of 50?1500 ng/mL with the correlation coefficient (r2) greater than 0.99, the quantitation limits (S/N=10) were 0.0005?0.02 mg/kg for each pesticides, the recoveries at the 3 levels of concentration addition were in the range of 62.3%?115.0%, and the relative standard deviations (n=6) were in the range of 0.76%?15.33%. Conclusion This method is sensitive, accurate, rapid and simple, and is suitable for rapid determination and verification of 59 kinds of pesticide residues in lotus seeds.