摘要
目的通过优化气相色谱和质谱条件,建立采用固相萃取(SPE)净化结合气相色谱-质谱法同时分析果蔬中27种农药残留的方法。方法样品匀浆后用乙腈超声提取盐析过滤,氮气吹干后用丙酮二氯甲院(1:1)复溶经无水硫酸钠过滤后,Cleanert PC/NH_2-SPE固相萃取柱净化氮吹浓缩正己烷定容。采用TG-5MS毛细管柱和质谱检测器测定内标法定量。结果 27种农药在50 min内完全分离在0.05~1.5 mg/L范围内线性良好相关系数R^2均>0.998,检出限为0.14~9.84μg/kg,平均加标回收率在77.6%~114.2%范围,相对标准偏差2.19%~9.18%。结论所建立的方法背景干扰少,净化效果好,简便、快速具有较高的准确度与精密度适用于果蔬中农药残留的测定。
Objective To found a method for the developed for determination of 27 pesticides residues in vegetables and fruits using solid-phase extraction（SPE） and gas chromatography/mass spectrometry based on optimal gas chromatography and mass spectrometry conditions.Methods The pesticides residues were extracted from homogenized vegetables and fruit samples with acetonitrile,and salted-out,filtrated,redissolved by acetone and dichloromethane（1：1） after dryed with nitrogen gas,then filtrated by anhydrous sodium sulfate,purified through Cleanert PC/NH_2-SPE column,concentrated by the nitrogen,and dissolved by n-hexane.The homogenized samples were detected by TG-5MS capillary column and gas chromatography/mass spectrometry,quantitatived analysis by internal standard method.Results The 27 kinds of pesticides were separated completely within 50 min,and the correlation coefficients within the range of 0.05-1.5 mg/L were more than 0.998.The minimum detection concentration were 0.14-9.84 μg/kg,the average recovery rates were 77.6%-114.2%and the relative standard deviation were 2.19%-9.18%.Conclusion This established method was simple,rapid with low background and highly accuracy and precision,and be suitable for determination of pesticide residues in vegetables and fruit.
作者
李亮
代飞飞
关晓晨
LI Liang DAI Fei-fei GUAN Xiao-chen(Department of Laboratory, Weifang Disease Control and Prevention Center, Weifang Shandong Province 261061, China)
出处
《中国城乡企业卫生》
2017年第1期55-59,共5页
Chinese Journal of Urban and Rural Enterprise Hygiene
基金
潍坊市卫生与计划生育委员会科研项目(2015007)
关键词
气相色谱/质谱
固相萃取
有机磷
氨基甲酸酯
拟除虫菊酯
GC-MS
Solid phase extraction-gas
Organic phosphorus pesticides
Carbamate pesticides
Pyrethroid pesticides
