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1.9~25.5μg/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、100μg/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。
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.
出处
《食品科学》
EI
CAS
CSCD
北大核心
2014年第24期301-307,共7页
Food Science
基金
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)
关键词
基质固相分散萃取
气相色谱-质谱
农药残留
蔬菜
solid phase dispersive extraction
gas chromatography-tandem mass spectrometry(GC-MS-MS)
pesticide residues
vegetable