摘要
选择氨基柱为固相萃取净化柱,以电喷雾(ESI)为离子源,正负离子切换多级反应离子检测(MRM)方式,建立了基质校正固相萃取液相色谱-串联质谱法(LC-MS/MS)测定食用菌中22种农药残留的分析方法。研究了不同固相萃取柱和洗脱剂对农药保留行为的影响,优化了净化方法、色谱分离条件和质谱条件。研究了平菇、香菇、杏鲍菇和蟹味菇的基质效应。22种农药在0.05～100μg/L(或0.1～200μg/L)范围内线性相关,相关系数为0.9874～0.9997,方法定量限为0.031～1.76μg/kg。除甲基硫菌灵和克螨特外,20种农药在4种食用菌中3个添加浓度的回收率在54.6%～128.0%,RSD为0.3%～29.0%之间,方法灵敏度高,选择性强。
By using NH2-SPE as the solid-phase extraction column and electrospray ionization（ESI） as the ion source,a method was developed for the determination of 22 pesticides residues in domestic fungus by solid-phase extraction and LC/MS/MS with MRM and matrix correction,in which the positive ions or negative ions are switched in the same scan time.The conditions of LC and MS for determination of 22 pesticides residues were optimized.The retention behavior of pesticides in different solid phase extraction cartridges and in various eluent solvent was studied.The optimal conditions for solid phase extraction clean-up and sample extraction method were described.There was a good linear relationship within the range of 0.05-100 μg/L（or 0.1-200 μg/L） by LC/MS/MS with MRM.The method quantitation limits were in the range of 0.031-1.76 μg/kg for 22 pesticides in domestic fungus.The matrix effects for 22 pesticides in pleurotus ostreatus,lentinus edodes,pleurotus eryngii and crab mushroom were considered.The correlation coefficients for 22 pesticides are in the range of 0.9874-0.9997.The recoveries of 20 pesticides from three spiked level were in the range of 54.6%-128.0% with RSD of 0.3%-29.0% for pleurotus ostreatus,leurotus eryngii,crab mushroom and lentinus edodes except thiophanate-methyl and propargite.The method has high sensitivity and selectivity.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2013年第8期1259-1263,共5页
Chinese Journal of Analytical Chemistry
关键词
固相萃取
食用菌
液相色谱-串联质谱法
农药残留
基质校正
Solid phase extraction
Domestic fungus
Liquid chromatography tandem mass spectrometry
Pesticides residues
Matrix correction
