Determination of Forbidden Pesticide Residues in Resinous Chinese Medi-cine by Gel Permeation Chromatography Combined with Gas Chroma-tography Tandem Mass Spectrometry
A gas chromatography tandem mass spectrometry(GC-MS/MS)was established for the determination of 24 forbidden pesticide residues in resinous Chinese medicine,based on gel permeation chromatography(GPC)cleanup.By comparing the purification effects of different pre-treatment methods,acetonitrile was selected to extract pesticide compounds from resinous Chinese medicine.After concentra-tion,the extracted solution was redissolved in ethyl acetate-cyclohexane solution(1∶1,V/V).BIO-Beads SX3(25 mm× 300 mm)gel puri-fication columns were used to purify the samples through gel permeation chromatography to separate and remove most impurities such as resins and pigments.The purified solution separated on a VF-5ms(30 m× 0.25 mm× 0.25 μm)capillary column,finally detected with elec-tron bombardment ionization source(EI)in selected ion monitoring(SIM)mode and quantified by internal standard method.The results showed that the 24 prohibited pesticides had a good linear relationship in a certain concentration range,the correlation coefficients(r)was greater than 0.99,the detection limit was 0.001～0.005 mg/kg.For typical olibanum sample matrices,the average recoveries at three spiked levels ranged from 66.7％～117.5％,with relative standard deviations(RSD)of 2.3％～12.5％.In this study,gel permeation chromatography technology was used as the purification method of resinous medicine,which overcame the defects of insufficient purification capacity of di-spersed solid phase extraction and solid phase extraction,solved the pollution and interference problems of resinous medicine impurities on the mass spectrometry system,improved the qualitative and quantitative accuracy,and has the characteristics of strong operability,high sen-sitivity and good repeatability.It can meet the high throughput detection requirements of prohibited pesticides in resinous medicine,and form an effective supplement of detection methods of prohibited pesticides in special matrix medicinal materials.
gel permeation chromatographygas chromatography tandem mass spectrometryresinous Chinese medicinepesticide residues
万方数据
维普
