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《Physical Testing and Chemical Analysis(Part B:Chemical Analysis)》 2019-03
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Simultaneous Determination of Neonicotinoid Insecticides and Their Metabolites in Honey by High Performance Liquid Chromatography-Tandem Mass Spectrometry with Dispersive Solid-Phase Extraction

HOU Jianbo;XIE Wen;QIAN Yan;WANG Peng;LEI Meikang;CHEN Yunyin;Technical Center of Zhejiang Entry-Exit Inspection and Quarantine Bureau;Zhejiang Academy of Science and Technology for Inspection and Quarantine;Zhejiang Lead Product Technic Co.Ltd.;College of Chemistry and Chemical Engineering,Zhejiang University of Technology;  
The honey sample(2.00 g) was added into in a centrifuge tube with a cover,and 100μL of isotope internal standard solution(200μg·L~(-1)) and 10 mL water were added.After mixing well by vortex,the mixture was made up to 20 mL with methanol,and mixed well,centrifuged at 8 500 r·min~(-1) for 5 min.0.50 mL of the supernatant was taken and diluted to 10.0 mL with methanol,and the mixture was mixed well by vortex,then centrifuged at 8 500 r·min~(-1) for 5 min.1.0 mL of the supernatant was transferred into a centrifuge tube containing a homogeneously mixed adsorbent(30 mg of N-propyl ethylenediamine,15 mg of C_(18) powder and 50 mg of anhydrous MgSO_4).After vortexing and mixing for adsorption purification,the tube was centrifuged at 8 500 r·min~(-1) for 5 min.All the supernatant was blowed to near dryness using nitrogen at 40 ℃,and the residue was disolved and made up to 1.0 mL with a mixture of methanol and 0.15%(volume fraction)formic acid solution(1+9).The solution was passed through a 0.22μm filter,and the filtrate was analyzed by liquid chromatographytandem mass spectrometry.Chromatographic separation was carried out using an Agilent Eclipse XDB-C_(18) column,with a mixture in varying proportions of 0.15% formic acid solution containing 5 mmol·L~(-1) ammonium acetate and methanol as mobile phase for gradient elution.Electrospray ion source,positive ion scanning mode and multireaction monitoring mode were used in the mass spectrometry,and the isotope dilution internal standard method and external standard method were used for quantification.The mass concentration of pyridoxine,dinotefuran,nitenpyram,thiame-thoxam,flonicamid,imidacloprid,clothianidin,chlorothiazide,acetamiprid,thiacloprid,4-(trifluoromethyl) nicotinamide and N-desmethylpyrazole,was linear within definite ranges,and the lower limits of determination(10 S/N) were between 2.5-12.5μg·kg~(-1).Tests for recovery was made by standard addition method to blank honey samples,giving results in the range of 79.9%-108%,and RSDs(n=6) were between1.7% and 15%.
【Fund】: 国家质检总局科技计划项目(2016IK280);; 浙江出入境检验检疫局科技计划项目(ZK201710X)
【CateGory Index】: O657.63;S896.1
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5 HOU Ru-yan,CAI Hui-mei,ZHANG Zheng-zhu and WAN Xiao-chun(College of Tea&Food Sicence and Technology,Key Laboratory of Tea biochemistry & biotechnology,Ministry of Agriculture,PRC,Anhui Agricultural University,Hefei 230036);Determination of neonicotinoid pesticide residues in vegetables and fruits with high-performance liquid chromatography with diode-array detection[J];分析试验室;2010-02
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6 LIU Hong-cheng,LI Qi-wan (Supervision & Testing Center for Farm Product Quality,Ministry of Agriculture,(Kunming),Kunming 650223; Institution of Qualification Standard and Test Technology,Yunnan Academy of Agriculture Science,Kunming 650223);Determination of Nicotine in Mushroom by a Fast Sample Preparation Method[J];分析科学学报;2012-01
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9 ZHANG Guiqun1,NIE Siqiao2,LONG Liping1,ZENG Dongqiang1,CHEN Jiuxing2,YANG Hui 3,CHEN Linglong4(1.College of Agriculture,Guangxi University,Nanning 530004,China;2.National Engineering Research Center for Agrochemicals,Hunan Research Institute of Chemical Industry,Changsha 410007,China;3.College of Chemistry and Chemical Engineering of Central South University,Changsha 410083,China;4.College of Chemistry and Chemical Engineering,Hunan Normal University,Changsha 410081,China);Determination of nitenpyram residue in cabbage and soil using gas chromatography[J];色谱;2010-11
10 LI Yan-fang1,LUO Hua-jian1,YE Yu-fei2,LI Liang2,LIANG Wei-qu1,HU Shan1,HUANG Hao1,CHEN Shi-li1(1.Agriculture Research Center of Dongguan,Dongguan 523086,China;2.Dongguan Supervision and Test Institution of Agricultural Produts Quality and Safety,Dongguan 523086,China);Gas chromatography with electron capture detector determination of organophosphorus, phenylpyrazolone and nicotine pesticides residues in cabbages[J];广东农业科学;2010-11
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