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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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【Citations】
Chinese Journal Full-text Database 5 Hits
1 WANG Dong;HOU Chuan-jin;ZHAO Er-cheng;JIA Chun-hong;School of Light Industry and Chemical Engineering,Dalian Polytechnic University;Institute of Plant Protection and Environment Protection,Beijing Academy of Agriculture and Forestry Science;;Determination of Neonicotinoid Residues in Honey by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry Combined with Salting-out Homogeneous Liquid-Liquid Extraction and Dispersive Solid-phase Extraction[J];分析测试学报;2015-06
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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
【Co-citations】
Chinese Journal Full-text Database 10 Hits
1 Nie Kun;Haidian District Institute of Products Quality Supervision and Inspection;;Determination of the Thiamethoxam in Vegetable by LC/MS/MS[J];食品工业;2015-11
2 LIU Songnan;ZHAO Xinying;DONG Xiaoqian;XU Wenwen;ZHAO Rong;Beijing Tea Qualify Supervision and Inspection Station;Beijing Centre for Physical and Chemical Analysis,Beijing Key Laboratory of Organic Materials Testing Technology &Quality Evaluation;;Determination of imidaclothiz in tea by QuEChERS cleanup and liquid chromatography-tandem mass spectrometry[J];色谱;2015-11
3 Zhang Xiaodong;Gong Daoxin;Wu Liang;He Wenbo;Yang Lihua;College of Resource and Environment,Hu'nan Agricultural University;Institute of Agricultural Environmental Protection,Hu'nan Agricultural University;;Determination of 3 neonicotinoid pesticide residues in paddy field with high performance liquid chromatography[J];农药学学报;2015-05
4 YAN Si-yue;LI Xing-hai;ZHAO Er-cheng;JIA Chun-hong;Institute of Plant Protection,Shenyang Agriculture University;Institue of Plant Protection and Environmental Protection,Beijing Academy of Agricultural and Forestry Science;;Determination of Organophosphorus Oesidues in Gas Ohromatography-Trandem Mass Spectrometry with Salting-out Homogeneous Liquid-Liquid Extraction and Dispersive Solid Phase Extraction[J];中国食品工业;2015-10
5 HUANG Yu-nan;LUO Jing;QIAO Cheng-kui;WANG Chao;PANG Tao;WU Feng-kui;CHENG Xin;Zhengzhou Fruit Research Institute,Chinese Academy of Agricultural Sciences,Laboratory of Quality and Safety Risk Assessment for Fruit(Zhengzhou);Therno Fisher Scientific;Center for Agri-Food Quality & Safety,Ministry of Agriculture,P.R.C;;HPLC Method for Detection of Thidiazuron Residues in Fruits and Vegetables[J];农药;2015-09
6 Zeng Guangfeng;Wang Zhiyuan;Chen Wenrui;Ding Bo;Wei Xiaoqun;Guangdong Entry-Exit Inspection and Quarantine Bureau;Guangdong Key Laboratory of Import and Export Technical Measures of Animal,Plant and Food;;Determination of Seven Kinds of Nicotinoid Insecticides in Vegetables by LC-Q-TOF-MS with QuEChERS[J];检验检疫学刊;2015-04
7 LIU Jisong;HU Cunzhong;LU Fan;SHI Haiyan;WANG Minghua;College of Plant Protection,Nanjing Agricultural University;Suke Agro-chemical of Jiangsu Province Co.Ltd;;Studies on the Degradation and Mobility of Dinotefuran in Soil[J];生态环境学报;2015-06
8 YU Lu;SONG Wei;L Yaning;ZHAO Muyu;ZHOU Fangfang;HU Yanyun;ZHENG Ping;College of Tea & Food Science and Technology,Anhui Agricultural University;Anhui Entry and Exit Inspection and Quarantine Bureau;Anhui Province Key Laboratory of Analysis and Detection for Food Safety;;Rapid determination of 204 pesticide residues in tea by ultra performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry[J];色谱;2015-06
9 ZHANG Hua;REN Pan-pan;CHEN Jian;WANG Li-zhi;HE Han-yi;OUYANG Yong-zhong;CHEN Huan-wen;Jiangxi Key Laboratory for Mass Spectrometry and Instrumentation,East China Institute of Technology;;Direct Analysis of Red Peppers Using Internal Extractive Electrospray Ionization Mass Spectrometry[J];质谱学报;2015-05
10 CAO Xiao-li;LIU Su-hua;LIU Zhong;YANG Xiao-qian;Ji'nan Centre for Disease Control and Prevention;;Determination of 62 pesticide residues in vegetables and fruits by gas chromatography-tandem mass spectrometry coupled with FDSPE[J];中国卫生检验杂志;2015-08
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2 YANG Dong-Dong;CONG Lu-Jing;TIAN Ming-Ming;WANG Ming-Hua;College of Plant Protection,Nanjing Agricultural University,Jiangsu Key Laboratory of Pesticide Science;;Determination of Three Neonicotinoid Pesticides Residues by High Performence Liquid Chromatography with Molecularly Imprinting Solid Phase Extraction[J];分析化学;2014-06
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4 BU Ming-nan1,2,SHI Zhi-hong1,KANG Jian2,3,FAN Chun-lin2,PANG Guo-fang2(1.College of Chemistry and Environmental Science,Hebei University,Baoding 071002,China;2.Chinese Academy of Inspection and Quarantine,Beijing 100123,China;3.College of Chemical and Environmental Engineering,Yanshan University,Qinhuangdao 066004,China);Simultaneous Determination of 72 Veterinary Drugs in Shrimp by Modified QuEChERS and High Performance Liquid Chromatography-Tandem Mass Spectrometry[J];分析测试学报;2012-05
5 XU Xiu-ying,SHI Hai-yan,WANG Ming-hua(The Plant Protection College of Nanjing Agricultural University,Nanjing 210095,China);Determination of Six Neonicotinoid Pesticides Residue in Rice by GC/MS[J];质谱学报;2012-02
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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