Citation: SUN Xiaojie, GUO Mengmeng, WANG Suyue, TAN Zhijun, LI Zhaoxin, ZHAI Yuxiu. Rapid determination of pesticide multiresidues in porphyra by dispersive solid-phase extraction coupled with online gel permeation chromatography-gas chromatography-mass spectrometry[J]. Chinese Journal of Chromatography, ;2014, 32(10): 1124-1130. doi: 10.3724/SP.J.1123.2014.06032 shu

Rapid determination of pesticide multiresidues in porphyra by dispersive solid-phase extraction coupled with online gel permeation chromatography-gas chromatography-mass spectrometry

1.
Yellow Sea Fisheries Research Institute, Chinese Academy of Fishery Sciences; Key Laboratory of Testing and Evaluation for Aquatic Product Safety and Quality, Ministry of Agriculture; National Center for Quality Supervision and Test of Aquatic Products, Qingdao 266071, China

Corresponding author: SUN Xiaojie, ZHAI Yuxiu,
Received Date: 23 June 2014

Fund Project: 国家自然科学基金项目(21207162) (21207162)农业部科技专项(2014FY230100). (2014FY230100)

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 (organochlorines, 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 pigments 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 programmed-temperature vaporizer of gas chromatography to improve the sensitivity of measurements. The results showed that the calibration curves were linear (r >0.995) in the range of 10-1000 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 pesticide residues in porphyra samples.
- dispersive solid-phase extraction,
- gel permeation chromatography-gas chromatography-mass spectrometry (GPC-GC/MS),
- pesticides,
- porphyra,
- multiresidues
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沈阳化工大学材料科学与工程学院沈阳 110142