气相色谱-串联质谱法测定蔬菜中氟乐灵等8种农药的残留量  

Determination of 8 kinds of pesticide residues in vegetables by gas chromatography-tandem mass spectrometry

作　　者：潘虎[1] 代艳娜[1] 张一帆[1] 白军平[1] PAN Hu DAI Yan-Na ZHANG Yi-Fan BAI Jun-Ping(Institute of Agricultural Product Quality Standard and Testing Research, Tibet Academy of Agricultural and Animal Husbandry Sciences, Lhasa 850032, Chin)

机构地区：[1]西藏自治区农牧科学院农业质量标准与检测研究所,拉萨850032

出　　处：《食品安全质量检测学报》2016年第7期2926-2930,共5页Journal of Food Safety and Quality

摘　　要：目的建立气相色谱-串联质谱法同时测定蔬菜中氟乐灵、嘧霉胺、甲霜灵、二甲戊灵、氟虫腈、溴螨酯、哒螨灵、苯醚甲环唑8种农药的残留量。方法样品经乙腈提取,以乙酸乙酯＋乙醇（9：1,V：V）作为洗脱液经CaTbon/NH2固相萃取柱净化,采用DB-5MS毛细管色谱柱分离;质谱采用电子轰击离子源模式电离,多反应监测模式测定。结果 8种农药在0.02-2.0 mg/L范围内呈现良好的线性关系,相关系数r为0.995-0.999;样品中添加0.02、0.20、2.0 mg/L3个浓度水平的8种农药混标工作液进行加标回收试验,平均回收率为83.2%-119.4%,RSD为1.8%-8.9%（n=5）,检出限为0.005-0.010mg/kg。结论该方法快速、准确,可适合蔬菜中多种农药残留的定量检测。Objective To establish a method for determination of 8 kinds of pesticides residues including trifluralin, pyrimethanil, metalaxyl, pendimethalin, fipronil, bromopropylate, pyridaben and difenoconazole in vegetables by gas chromatography-tandem mass spectrometry. Method Samples were extracted with acetonitrile, cleaned up with solid phase extration column of Carbon/NH2, and separated by DB-SMS column. Electron ionization （EI） mode and multiple reaction monitoring mode （MRM） were used in mass spectrometry. Results Eight kinds of pesticides had a good linear relationship in the range of 0.02-2.0 mg/L with correlation coefficient of 0.995-0.999. The mean recoveries spiked at 3 levels of 0.02, 0.20, and 2.0 mg/L in samples were in the range of 83.2%-119.4% with the relative standard deviations of 1.8%-8.9%（n=5）, and the limits of detection were in the range of 0.005-0.010 mg/kg. Conclusion The method is rapid and accurate, which can be applied for the quantitative detection of multi-pesticide residues in vegetables.

关 键 词：农药残留 气相色谱-串联质谱法 蔬菜 

分 类 号：O657.63[理学—分析化学] TS255.7[理学—化学]