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

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

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，比较了同相萃取（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0．01～10mg／L范围内线性关系良好，相关系数大于0．997。在0．01～1．0mg／kg添加水平范周内，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）0．001～0．01mg／kg之间，定量检出限（LOQ）为0．005～0．05mg／kg，相对标准偏差小于10％；MLLE法为LOD在0．02～0．10mg／kg，LOQ为0．06～0．30mg／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。

A multi-residue method has been developed for the confirmation and quantitation of 19 pesticides in red grape wine. Micro liquid-liquid extraction （LEE） 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.