MAE在线GPC-GC-MS/MS法测定板栗中20种有机磷农药残留  

Determination of 20 organophosphorous pesticide residues in chestnut by on-line GPC-GC-MS/MS using MAE

作　　者：席慧[1] 杨振兴[1,2] 张帆[1,3] 

机构地区：[1]长沙环境保护职业技术学院,湖南长沙410004 [2]湖南农业大学食品学院,湖南长沙410004 [3]湖南省检验检疫科学技术研究院,湖南长沙410004

出　　处：《湖南林业科技》2015年第4期56-61,共6页Hunan Forestry Science & Technology

基　　金："十二五"国家科技支撑计划(2012BAK08B01)

摘　　要：先以乙腈为提取溶剂,采用微波辅助萃取技术（MAE）对板栗样品中20种有机磷农药进行萃取（前处理）,然后将提取液经分散固相萃取净化,除去样品中大部分的脂肪和甾醇等干扰基质,再经在线GPC/GC—MS—MS在多反应监测模式（MRM）下进行检测和确证,建立了板栗中20种有机磷农药残留量的在线GPC—GC—MS/MS快速测定方法。测定结果表明：20种有机磷农药在0.01~0.20 mg/kg范围内的加标平均回收率为71.5%（104.0%,相对标准偏差为3.4%~9.4%。该方法准确、快速、净化效果好。In this study,an analytical method has been developed for the determination of 20 organophosphorous pesticides in chestnut. Chestnut were extracted with acetonitrile using microwave-assisted extraction technique（ MAE） and cleaned up using dispersive solid phase extraction（ DSPE） to remove most fats and sterols in samples,after cleaned using online gel permeation chromatography（ GPC）,the 20 target organophosphorous pesticides were rapidly detected by gas chromatography-tandem mass spectrometry（ GC-MS / MS）. The average recoveries of 20 target pesticides in spiked chestnut（ from 0. 01 to 0. 20 mg / kg） ranged from 71. 5% to 104. 0% with the relative standard deviation ranged from3. 4 % to 9. 4 %. The developed method is accurate,quick,and with high purifying efficiency,it provided technical reference for the quality and export of the chestnut.

关 键 词：微波萃取 在线凝胶渗透色谱—气相色谱/质谱 板栗 有机磷农药 

分 类 号：O652.62[理学—分析化学] S481.8[理学—化学]