葡萄酒中17种残留农药的固相萃取-气相色谱/负化学离子源质谱测定方法研究

建立了葡萄酒中17种残留杀虫剂和杀菌剂的气相色谱～负化学离子源质谱（GC—NCI／MS）测定方法。采用C18。固相萃取小柱对葡萄酒中的残留农药进行富集，进一步完成萃取和净化，农药经乙酸乙酯洗脱后供GC—NCI／MS测定，采用基质匹配标准溶液外标法定量。验证实验表明，各农药在10-200μg／L浓度范围内线性关系良好，该方法定量检测限（S／N〉10）为5-20μg/L，在20μg，L和50μg／L处的加标回收率为70．1％-119．0％，相对标准偏差为3．5％-9．4％。该方法前处理简便快速，所采用的检测技术选择性和灵敏度高，适合葡萄酒中残留农药的测定．应用前景广阔。

Determination of 17 Kinds of Pesticide Residues in Grape Wine by Solid Phase Extraction-Gas Chromatography/Negative Chemical Ionization Mass Spectrometry

A method has been developed for the determination of 17 kinds of pesticide residues in grape wine by solid phase extraction-gas chromatography/negative chemical ionization mass spectrometry(GC-NCI/MS).The pesticide residues in wine samples were extracted and purified by C18 SPE column,eluted with ethyl acetate and detected with GC-NCI/MS.The quantification was carried out by matrix-matched external standard curve,the calibration curves showed good linearity within the concentrations of 10 to 200 μg/L.The limit of quantification(LOD,S/N>10) were 5～20 μg/L.Recoveries spiked levels of 20 and 50 μg/L ranged from 70.1 % to 119.0 %,with the relative standard deviation of 3.5 %～9.4 %.Such method is simple,fast and sensitive,and is suitable for the determination of pesticide residues in grape wine.