微液液提取或固相萃取法净化、气相色谱-质谱联用检测葡萄酒中19种农药多残留

建立了红葡萄酒中19种农药多残留的气相色谱-质谱联用选择离子模式进行监测的检测方法,比较了固相萃取(SPE)和微液液提取(MLLE)两种前处理方法并考察了基质效应。两种方法在0.01~10 mg/L范围内线性关系良好,相关系数大于0.997。在0.01~1.0 mg/kg添加水平范围内,SPE法的平均添加回收率在77.8%~109.1%之间(四螨嗪为137.5%);MLLE法的平均添加回收率在83.3%~116.7%之间(四螨嗪为43%)。SPE法的最低检出限(LOD)0.001~0.01 mg/kg之间,定量检出限(LOQ)为0.005~0.05 mg/kg,相对标准偏差小于10%;MLLE法为LOD在0.02~0.10 mg/kg,LOQ为0.06~0.30 mg/kg,相对标准偏差小于14%。所有目标化合物均存在基质增强效应,可用基质匹配标准溶液来减少其对测定结果的影响。

Determination of 19 Multi-residue Pesticides in Grape Wine by Gas Chromatography-Mass Spectrometry with Micro Liquid-liquid Extraction and Solid Phase Extraction

A multi-residue method has been developed for the confirmation and quantitation of 19 pesticides in red grape wine.Micro liquid-liquid extraction(LLE) and solid phase extraction(SPE) were compared and gas chromatography-electron ionization mass spectrometry was used for the detection.Recoveries for SPE and micro LLE methods were found in the range of 77.8%-109.1%(137.5% for clofentezine) and 83.3%-116.7%(43% for clofentezine) with RSDs <14%,respectively.For the SPE and micro LLE methods,LODs ranged from 0.001 to 0.01 mg/kg and 0.02 to 0.10 mg/kg,while LOQs ranged from 0.005 to 0.05 mg/kg and 0.06 to 0.30 mg/kg,respectively,depending on the sensitivity of each compound.All of the targets had matrix enhancement effect,which could be reduced by using matrix-matched calibration solutions.