液相色谱-质谱联用检测蒲公英茶中的乙酰甲草胺

Determination of Diethatyl-Ethyl in Dandelion by Liquid Chromatography-Mass Spectrometer

目的:为了更有效地对我国蒲公英茶的质量和安全性进行监管,建立液相色谱-质谱联用检测蒲公英茶中的乙酰甲草胺的方法。方法:干燥后的蒲公英茶试样用含0.1%甲酸的乙腈溶液提取、脱色净化,离心,过0.22μm微孔滤膜,用液相色谱质谱法检测。采用C18(150 mm×4.6 mm,5μm)液相色谱柱分离,采用ESI+、MRM模式检测。结果:乙酰甲草胺浓度在0.1~100.0μg·L^(-1),曲线方程为y=2950x+89785,相关系数r=0.997,线性关系良好;在0.5μg·kg^(-1)、10.0μg·kg^(-1)、50.0μg·kg^(-1)3个添加水平下,乙酰甲草胺的平均回收率在99.06%,相对标准偏差为9.6%。结论:使用液相色谱-质谱联用检测蒲公英茶中的乙酰甲草胺的方法快捷,准确度、精密度好,可以满足蒲公英茶中乙酰甲草胺残留的定性和定量检测。

Objective:In order to effectively supervise the quality and safety of Chinese dandelion tea,a method for the detection of diethatyl-ethyl in dandelion by liquid chromatography-mass spectrometer was established.Method:The dried dandelion tea sample was extracted with acetonitrile solution containing 0.1%formic acid,decolorized and purified,centrifuged,passed through a 0.22μm microporous filter membrane,and detected by liquid chromatography mass spectrometry.Using C18(150 mm×4.6mm,5μm)liquid chromatography column separation and detection using ESI+and MRM modes.Result:The linear relationship of diethatyl-ethyl in dandelion matrix was good in the concentration range of 0.1~100.0μg·L^(-1).The curve equation was y=2950x+89785,the correlation coefficient r=0.997.The average recovery of acetolachlor was 99.06%with a mean relative standard deviation of 9.6%at 0.5μg·kg^(-1),10.0μg·kg^(-1),and 50.0μg·kg^(-1).Conclusion:The method of determination of diethatyl-ethyl in dandelion by liquid chromatography-mass spectrometer is fast,accurate and accurate,and can satisfy the qualitative and quantitative determination of diethatyl-ethyl residues in dandelion.