论文部分内容阅读
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5~500ng/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2.0μg/kg和5.0μg/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 liquid chromatography-tandem mass spectrometry (LC-MS / MS) method for the determination of 16 carbamate pesticides and their metabolites (aldicarb, aldicarb sulfoxide, aldicarb sulfoxide, Carbaryl, carbofuran, diethylmycin, sec-butyl, indoxacarb, isoprocarb, methomyl, trimethoprim, trimethoprim, pirimicarb and propoxur). Methods The samples were extracted with 0.1% glacial acetic acid - acetonitrile. The extracts were filtered, concentrated, and purified by a graphitized carbon black / amino solid phase extraction cartridge. The multi-reaction monitoring (MRM) Qualitative and quantitative analysis. Results 16 kinds of carbamate pesticides showed a good linearity in the concentration range of 5 ~ 500ng / mL. The detection limits and quantitative limits of 16 pesticides in apple, spinach, yam, rice, soybean and ginger were 2.0 μg / kg and 5.0 μg / kg, respectively, and were spiked at low, medium and high levels The rates ranged from 71.0% to 108.0%, and RSDs (relative standard deviations) ranged from 2.03% to 11.30%. Conclusion The method is simple and rapid, and its sensitivity, accuracy and precision can meet the requirements of pesticide residue analysis.