液相色谱-串联质谱法测定植物源性食品中 16种氨基甲酸酯类农药及其代谢物
目的 建立液相色谱-串联质谱法测定植物源性食品中16种氨基甲酸酯类农药及其代谢物(涕灭威、涕灭威亚砜、涕灭威砜、灭害威、恶虫威、甲萘威、克百威、乙霉威、仲丁威、茚虫威、异丙威、灭多威、速灭威、杀线威、抗蚜威和残杀威)残留量的方法。方法 样品用0.1%冰醋酸-乙腈提取, 提取液经过滤、浓缩后用石墨化炭黑/氨基固相萃取柱净化, 采用多反应监测(multi-reaction monitoring, MRM)正离子扫描模式进行准确的定性和定量分析。结果 16 种氨基甲酸酯类农药在5~500 ng/mL浓度范围内均呈良好线性。16种农药在苹果、菠菜、山药、大米、大豆和生姜6种基质中的检出限和定量下限为2.0 μg/kg和5.0 μg/kg, 在低、中、高3 个水平的加标回收率为71.0%~108.0%之间, RSDs (relative standard deviations)为2.03%~11.30%。结论 该方法简单快速,其灵敏度、准确度和精密度均能满足农药残留分析的要求。
Objective To establish a high pressure liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method for determination 16 kinds of carbamate pesticides and their metabolites (aldicarb, aldicarb-sulfoxide, aldicarb-sulfone, aminocarb, bendicarb, carbaryl, carbofuran, diethofencarb, fenobucarb, indoxacarb, isoprocarb, methomyl, metolcarb, oxamyl, pirimicarb and propoxur) in plant-derived foodstuffs. Methods Samples were extracted with 0.1% formic acid-acetonitrile solution. After concentrated, the solution was cleaned up with solid-phase extraction (SPE) column of envi-Carb/NH2, the mode of multi-reaction monitoring positive ion scanning was adopted for both the quantitative and qualitative analyses. Results Calibration curves showed a good linearity over the range of 5~500 ng/mL. The limits of detection (LOD) were 2.0 μg/kg and the limits of quantification (LOQ) were 5.0 μg/kg for all the 16 pesticides spiked in apple, spinach, Chinese yam, rice, soybean and ginger, respectively. The mean recoveries at three spiked concentration levels (low, middle, high) were in the range of 71.0%~108.0% with the relative standard deviations (RSDs) from 2.03% to 11.3%. Conclusion This method is simple and fast, and its sensitivity, accuracy and precision can satisfy the requirement of pesticide residue analysis.
标题：液相色谱-串联质谱法测定植物源性食品中 16种氨基甲酸酯类农药及其代谢物
英文标题：Determination of 16 carbamate pesticides and metabolite residues in plant-derived foodstuffs by high pressure liquid chromatography-tandem mass spectrometry
作者：
王敬 河北出入境检验检疫局技术中心
陈瑞春 河北出入境检验检疫局技术中心
郭春海 河北出入境检验检疫局技术中心
窦彩云 河北出入境检验检疫局技术中心
中文关键词:液相色谱-串联质谱法,氨基甲酸酯类农药,植物源性食品,残留,
英文关键词:high pressure liquid chromatography-tandem mass spectrometry (HPLC-MS/MS),carbamate pesticides,plant-derived foodstuffs,residue,
发表日期：2013-09-17
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