摘要
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.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2007年第10期1430-1434,共5页
Chinese Journal of Analytical Chemistry
基金
农业部引进项目984专项支持(No.2005-Z34)
关键词
微液液提取
同相萃取
气相色谱-质谱联用
红葡萄酒
多残留
基质效应
Micro liquid-liquid extraction, solid phase extraction, gas chromatography-electron ionizationmass spectrometry, red grape wine, multi-residue, matrix effect