超高效液相色谱–串联质谱法测定香菇中29种农药残留

Determination of 29 pesticide residues in lentinus edodes by ultra performance liquid chromatography–tandem mass spectrometry

建立同时测定香菇中29种农药残留的超高效液相色谱-串联质谱(UPLC-MS/MS)方法。样品以0.1%甲酸-乙腈溶液为提取剂,用氨基固相萃取柱净化,经浓缩、复溶后进行测定。采用C18柱分离,以0.1%甲酸溶液和乙腈作为流动相,多反应监测(MRM)模式检测,用基质匹配标准溶液外标法定量。29种农药在各自的质量浓度范围内与其色谱峰面积呈良好的线性关系,相关系数大于0.995,方法检出限为0.0001~0.002mg/kg。在0.02,0.05,0.1mg/kg3个浓度水平进行加标回收试验,平均回收率为81.3%~97.9%,测定结果的相对标准偏差为2.0%~8.4%(n=6)。该方法前处理过程简便,检测时间短,测定结果准确稳定,适合大批量香菇样品中多农药残留的检测,对于香菇的市场准入和监测有着积极意义。

In order to detect pesticide residues in lentinous edodes rapidly and effectively,a method was developed for simultaneous determination of 29 pesticide residues by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS).The samples were extracted with 0.1% formic acid-acetonitrile solution,and cleaned up by amino solid phase extraction column.The purified liquid was evaporated and redissolved for detection.The analytes were separated by C18 column,ormic acid solution and acetonitrile solution were used as the mobile phase,and finally detected by multiple reaction monitoring (MRM) mode.Quantification analysis was achieved by external standard method with the matrix matches of standard solution.The mass concerntration of 29 pesticides had good relationship in the linear range with the linear correlation coefficients of more than 0.995.The limits of quantitation for the 29 pesticides ranged from 0.000 1-0.002 mg/kg.The average recoveries at spiked levels of 0.02,0.05,0.1 mg/kg ranged from 81.3% to 97.9% with relative standard deviations of 2.0%-8.4%(n=6).The method is suitable for the detection of multi-pesticide residues in large quantities of lentinus edodes samples with the simple pretreatment process,accurate and stable detection results,and the short analysis time.This method has positive significance for market access and monitoring of lentinous edodes.