气相色谱-飞行时间质谱联用快速筛查桃中的25种农药残留  

Rapid Screening of 25 Pesticide Residues in Peach by Gas Chromatography-time of Flight Mass Spectrometry

作　　者：马智玲[1] 李凌云[2] 刘新艳[2] 魏长宾[1] 刘玉革[1] 刘肃[2] 方佳[3] 

机构地区：[1]农业部热带果树生物学重点实验室中国热带农业科学院南亚热带作物研究所,广东湛江524091 [2]农业部蔬菜品质监督检验测试中心中国农业科学院蔬菜花卉研究所,北京100081 [3]中国热带农业科学院,海南海口571101

出　　处：《热带作物学报》2015年第4期804-812,共9页Chinese Journal of Tropical Crops

基　　金：中国热带农业科学院南亚热带作物研究所中央级公益性科研院所基本业务费专项(No.1630062015013);中国热带农业科学院大型仪器设备共享中心

摘　　要：应用分散固相萃取（DSPE）与分散液液微萃取（DLLME）相结合的样品前处理技术,与气相色谱-飞行时间质谱（GC-TOF/MS）联用,建立了同时快速筛查桃中25种农药残留的分析方法,实验考察了2种萃取方法中影响净化和萃取效率的各个因素,并建立了飞行时间质谱农药筛查数据库。结果表明：在优化的实验条件下,25种农药在一定的浓度范围内线性良好,相关系数（r）均大于0.98;桃空白基质在10、30、50μg/kg 3个不同的添加浓度下,农药的平均回收率为64.9%~119.8%,相对标准偏差（RSD）为3.5%~22.1%,方法的检出限（LOD,S/N≥3）和定量限（LOQ,S/N≥10）范围分别为0.01~12.30μg/kg和0.1~36.7μg/kg。In the article, a simple and efficient method for rapidly screening of 25 pesticide residues simultaneously in peach was developed by using dispersive solid phase extraction（DSPE）and dispersive liquid-liquid microextraction（DLLME） coupled with gas chromatography-time of flight（GC-TOF/MS）. Parameters affecting purification and extraction efficiency in both procedures were investigated and optimized to achieve the best extraction efficiency. Database of GC-TOF-MS for the screening of pesticides was also established. In the optimum conditions, the results showed that all the 25 pesticides had good linearity in a certain range and the correlation coefficient（r） was higher than 0.98. The average recoveries for the most of the pesticides in peach matrices were in the range of 64.9%-119.8% at three spiked levels of 10 μg/kg, 30 μg/kg, 50 μg/kg, with RSDs of 3.2%-22.1%. The limits of detection（LOD, S/N≥3）and LOQ（S/N≥10） of the method were 0.01-12.30 μg/kg and 0.1-36.7 μg/kg respectively.

关 键 词：桃 农药多残留 DSPE DLLME GC-TOF/MS 

分 类 号：S481.8[农业科学—农药学]