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基质固相分散萃取-气相色谱-串联质谱法同时测定蔬菜中195 种农药残留
引用本文:李 蓉,卢俊文,杨 芳,张朋杰,李拥军,谢建军,储大可. 基质固相分散萃取-气相色谱-串联质谱法同时测定蔬菜中195 种农药残留[J]. 食品科学, 2014, 35(24): 301-307. DOI: 10.7506/spkx1002-6630-201424058
作者姓名:李 蓉  卢俊文  杨 芳  张朋杰  李拥军  谢建军  储大可
作者单位:1.中山出入境检验检疫局,广东 中山 528403;2.中山市农产品质量监督检验所,广东 中山 528400;3.广东出入境检验检疫局,广东 广州 510623;4.广东药学院,广东 中山 528400
基金项目:中山市科技计划—农业科技攻关计划项目(20103A190);中山市科技发展专项(2013A3FC0251)
摘    要:目的:建立一种蔬菜中195 种农药的气相色谱-质谱检测方法。方法:样品用乙酸乙酯匀浆提取后,经基质固相分散萃取法净化,气相色谱-质谱仪的选择反应监测模式-进行测定,内标法定量。结果:在0.01~1.00 mg/L质量浓度范围内,所有农药的线性相关系数均大于0.99,方法的定量限范围为1.9~25.5 μg/kg。分别在菜心、生菜、黄瓜、芹菜、土豆等蔬菜中进行3 个添加水平(10、20、100 μg/kg)实验,平均回收率为37.6%~136.7%,相对标准偏差为0.2%~15.3%。结论:该方法快速、灵敏、准确、高通量,具有良好的回收率和稳定性,较好地解决了样品本底成分复杂带来的基质干扰,适用于蔬菜中195 种农药残留量的快速测定。

关 键 词:基质固相分散萃取  气相色谱-质谱  农药残留  蔬菜  

Simultaneous Determination of 195 Pesticide Residues in Vegetables Using Solid Phase Dispersive xtraction-Gas Chromatography-Tandem Mass Spectrometry
LI Rong,LU Jun-wen,YANG Fang,ZHANG Peng-jie,LI Yong-jun,XIE Jian-jun,CHU Da-ke. Simultaneous Determination of 195 Pesticide Residues in Vegetables Using Solid Phase Dispersive xtraction-Gas Chromatography-Tandem Mass Spectrometry[J]. Food Science, 2014, 35(24): 301-307. DOI: 10.7506/spkx1002-6630-201424058
Authors:LI Rong  LU Jun-wen  YANG Fang  ZHANG Peng-jie  LI Yong-jun  XIE Jian-jun  CHU Da-ke
Affiliation:1. Zhongshan Entry-Exit Inspection and Quarantine Bureau, Zhongshan 528403, China;2. Zhongshan Quality Supervision and Inspection Institute of Agricultural Products, Zhongshan 528400, China;3. Guangdong Entry-Exit Inspection and Quarantine Bureau, Guangzhou 510623, China;4. Guangdong Pharmaceutical University, Zhongshan 528400, China
Abstract:Objective: To develop a method for the determination of 195 pesticide residues in vegetables using gas
chromatography with tandem mass spectrometry (GC-MS-MS) under a selected reaction monitoring (SRM) mode. Methods:
The target compounds were extracted from samples with ethyl acetate and the extract was cleaned up by off-line solid phase
dispersive extraction technique. The analytes were quantified by an internal standard method. Results: In the linear range
(0.01–1.00 mg/L), the correlation coefficient for each pesticide was higher than 0.99. The average recoveries at three spiked
levels (10, 20 and 100 μg/kg) varied from 37.6% to 136.7% with relative standard deviations (RSDs) between 0.2% and 15.3%.
The limits of quantification (LOQ) (signal/noise ratio = 10) were 1.9–25.5 μg/kg. Conclusion: The method is rapid, sensitive,
accurate and high throughput, without matrix interference and suitable for the analysis of 195 pesticide residues in vegetables.
Keywords:solid phase dispersive extraction  gas chromatography-tandem mass spectrometry (GC-MS-MS)  pesticide residues  vegetable  
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