色谱Issue(10)：1124-1130,7.DOI:10.3724/SP.J.1123.2014.06032
分散固相萃取-在线凝胶色谱-气相色谱-质谱联用法快速检测紫菜中的农药多残留
Rapid determination of pesticide multiresidues in porphyra by dispersive solid-phase extraction coupled with online gel permeation chromatography-gas chromatography-mass spectrometry
摘要
Abstract
A rapid method for the simultaneous identification and quantification of pesticide multiresidues in porphyra was developed using gel permeation chromatography( GPC)coupled to gas chromatography-mass spectrometry( GPC-GC/MS). Nineteen pesticides( organochlo-rines,organophosphoruses,triazines and pyrethroids)were selected as the target analytes. The pretreatment method was applied consisting of organic solvent extraction followed by dispersive solid-phase extraction with graphitized carbon black ( GCB ) and primary secondary amine ( PSA)adsorbents. GPC was also employed online to remove the large molecules such as pig-ments and lipids. The quantitative analysis was carried out by external standard method using gas chromatography coupled with mass spectrometry in selective ion monitoring( SIM)mode. Moreover,a large volume of sample was allowed to be injected using the program of GPC pro-grammed-temperature vaporizer of gas chromatography to improve the sensitivity of measure-ments. The results showed that the calibration curves were linear( r﹥0. 995)in the range of 10-1 000 μg/L for all the pesticides. The limits of detection( LODs)for the pesticides in porphyra were from 0. 005 to 0. 03 mg/kg,and the average recoveries were between 70% and 120%. The advantages of the method are simple,sensitive and shorter operation time for analysis of pesti-cide residues in porphyra samples.关键词
分散固相萃取/凝胶色谱-气相色谱-质谱/农药/紫菜/多残留Key words
dispersive solid-phase extraction/gel permeation chromatography-gas chromatog-raphy-mass spectrometry( GPC-GC/MS)/pesticides/porphyra/multiresidues分类
化学化工引用本文复制引用
孙晓杰,郭萌萌,王苏玥,谭志军,李兆新,翟毓秀..分散固相萃取-在线凝胶色谱-气相色谱-质谱联用法快速检测紫菜中的农药多残留[J].色谱,2014,(10):1124-1130,7.基金项目
国家自然科学基金项目（21207162）；农业部科技专项（2014FY230100）． （）
