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| Determination of Pyrethroid Pesticide Residues in Tobacco Leaf by Magnetic Solid Phase Extraction Combined with GC－MS Based on Magnetic Composite |
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| DOI： |
| KeyWord:cyclodextrin magnetic composite magnetic solid-phase extraction pyrethroid tobacco leaf |
| Author | Institution |
| YANG Yu-ming，LIU Yuan-chen，LIU Zhi-min，LI Jiao， SI Xiao-xi， LIN Tao， LIU Hong-cheng， XU Zhi-gang |
1. Faculty of Science， Kunming University of Science and Technology， Kunming ， China; 2. R&D Center of China Tobacco Yunnan Industrial Co. Ltd.， Kunming ， China; 3. Institute of Quality Standard and Testing Technology， Yunnan Academy of Agriculture Science， Kunming ， China |
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| Abstract: |
| This paper is related to a method that magnetic composite material （Fe3O4@SiO2@β-CD） based on β-cyclodextrin（β-CD）was established by magnetic solid phase extraction－gas chromatography－mass spectrometry for determination of four pyrethroid pesticide residues in tobacco： bifenthrin， fenpropathrin， cyfluthrin and deltamethrin. The adsorption capacity for pyrethroid pesticides of composite materials bonded with different cyclodextrin derivatives， namely Fe3O4@SiO2@α-CD， Fe3O4@SiO2@β-CD and Fe3O4@SiO2@γ-CD， were studied and compared. The results of extraction experiments showed that the Fe3O4@SiO2@ β-CD had the superior extraction rate for four target analytes. The prepared Fe3O4@SiO2@β-CD was identified via scanning electron microscope， infrared spectroscopy， X-ray diffractometer and microporous adsorption material analysis tester. The effects of extraction time， desorption time， desorption solvent， solution pH value and salt ion concentration on the extraction performance of magnetic composite materials were investigated. Furthermore， the extraction capacity experiment was carried out to investigate the effect of β-CD modified magnetic composite material on the extraction performance. The results showed that the extraction capacity of Fe3O4@SiO2@β-CD material was enhanced significantly compared with unmodified Fe3O4 and Fe3O4@SiO2. An analytical method based on β-cyclodextrin magnetic composite magnetic solid phase extraction coupled with gas chromatography－mass spectrometry for the analysis of pyrethroid pesticide residues was established. The results show that the magnetic composite material Fe3O4@SiO2@β-CD can be used for the extraction and analysis of four pyrethroid pesticide residues in tobacco leaves. The linear ranges of four analytes are 0.1－3.0 mg/kg and the linear correlation coefficients are higher than 0.998. The detection limits are all 0.03 mg/kg. The recoveries of standard addition for four analytes are between 65.9% and 107%， and the relative standard deviations（n = 3） are between 0.70% and 12%. |
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