液相色谱-串联质谱法测定白芍禁用农药残留

Determination of prohibited pesticide residues in white peony by liquid chromatography-tandem mass spectrometry

建立液相色谱-串联质谱法(LC-MS/MS)同时测定白芍中29种禁用农药残留的分析方法。白芍粉末试样经乙腈浸泡过夜后超声波提取,采用固相萃取小柱净化,经LC-MS/MS正离子模式扫描分析29种禁用农药残留。结果表明,29种禁用农药的线性相关系数良好(R2>0.9951),检出限为0.0001~0.0300 mg/kg,定量限为0.0003~0.0900 mg/kg;在0.01~0.50 mg/kg的加标水平下,29种禁用农药的回收率为66.8%~108.4%,相对标准偏差(n=6)为0.9%~12.3%。此方法成功应用于白芍质控样品中29种禁用农药的定性和定量分析,定性准确,定量结果在质控证书不确定度范围内,适用于白芍中29种禁用农药的残留分析。

A liquid chromatography-tandem mass spectrometry(LC-MS/MS)method was established for the simultaneous determination of 29 prohibited pesticide residues in the white peony.The white peony powder sample was soaked overnight in acetonitrile and extracted by ultrasound.The solid phase extraction column was used for purification,and 29 prohibited pesticide residues were analyzed by LC-MS/MS positive ion mode scanning.The results showed that the linear correlation coefficient of 29 prohibited pesticides was good(R2>0.9951),with a detection limit of 0.0001~0.0300 mg/kg and a quantitative limit of 0.0003~0.0900 mg/kg;at the spiked level of 0.01~0.50 mg/kg,the recovery rates of 29 prohibited pesticides were 66.8%~108.4%,and the relative standard deviation(n=6)was 0.9%~12.3%.This method had been successfully applied to the qualitative and quantitative analysis of 29 prohibited pesticides in the quality control samples of the white peony.The qualitative accuracy was accurate,and the quantitative results were within the uncertainty range of the quality control certificate.It was suitable for the residual analysis of 29 prohibited pesticides in the white peony.