title: Multi-residue method for determination of seven neonicotinoid insecticides in grains using dispersive solid-phase extraction and dispersive liquid-liquid micro-extraction by high performance liquid chromatography.
abstract: A method using dispersive solid-phase extraction and dispersive liquid-liquid micro-extraction cleanup followed by high performance liquid chromatography (HPLC) has been established for determination of seven neonicotinoid insecticides residues in grains including brown rice, maize, millet and oat. Based on an appraisal of the characteristics of HPLC, validation experiments were conducted for seven neonicotinoid insecticides. In the method, dispersive solid-phase extraction was carried out using PSA and bonded C18 coupled with graphitised carbon black with acetonitrile as the eluted solvent. In the linear range of each pesticide, the correlation coefficient was R(2) ≥ 0.99. At the low, medium and high three fortification levels of 0.05-0.8 mg kg(-1), recoveries fell within 76-123%. The relative standard deviation was between 0.9% and 12.6% for seven neonicotinoid pesticides. Low limits of detection (0.002-0.005 mg kg(-1)) and quantification (0.007-0.018 mg kg(-1)) were readily achieved with this method for all tested pesticides.
authors.affiliation: Department of Food Sciences, School of Food Science and Engineer, Harbin Institute of Technology, No. 73 Huanghe Road, Nangang District, Harbin 150090, Heilongjiang Province, PR China.
authors.forename: P
authors.initials: P
authors.lastname: Wang
authors.affiliation: Department of Food Sciences, School of Food Science and Engineer, Harbin Institute of Technology, No. 73 Huanghe Road, Nangang District, Harbin 150090, Heilongjiang Province, PR China; Key Laboratory of Agro-product Quality and Safety, Institute of Quality Standard & Testing Technology for Agro-product, Chinese Academy of Agricultural Sciences, No. 12 South Street, Zhongguancun, Haidian District, Beijing 100081, Beijing Province, PR China.
authors.forename: X
authors.initials: X
authors.lastname: Yang
authors.affiliation: Key Laboratory of Agro-product Quality and Safety, Institute of Quality Standard & Testing Technology for Agro-product, Chinese Academy of Agricultural Sciences, No. 12 South Street, Zhongguancun, Haidian District, Beijing 100081, Beijing Province, PR China.
authors.forename: J
authors.initials: J
authors.lastname: Wang
authors.affiliation: Department of Food Sciences, School of Food Science and Engineer, Harbin Institute of Technology, No. 73 Huanghe Road, Nangang District, Harbin 150090, Heilongjiang Province, PR China.
authors.forename: J
authors.initials: J
authors.lastname: Cui
authors.affiliation: Department of Food Sciences, School of Food Science and Engineer, Harbin Institute of Technology, No. 73 Huanghe Road, Nangang District, Harbin 150090, Heilongjiang Province, PR China.
authors.forename: A J
authors.initials: AJ
authors.lastname: Dong
authors.affiliation: Department of Food Sciences, School of Food Science and Engineer, Harbin Institute of Technology, No. 73 Huanghe Road, Nangang District, Harbin 150090, Heilongjiang Province, PR China.
authors.forename: H T
authors.initials: HT
authors.lastname: Zhao
authors.affiliation: Department of Food Sciences, School of Food Science and Engineer, Harbin Institute of Technology, No. 73 Huanghe Road, Nangang District, Harbin 150090, Heilongjiang Province, PR China.
authors.forename: L W
authors.initials: LW
authors.lastname: Zhang
authors.affiliation: Department of Food Sciences, School of Food Science and Engineer, Harbin Institute of Technology, No. 73 Huanghe Road, Nangang District, Harbin 150090, Heilongjiang Province, PR China.
authors.forename: Z Y
authors.initials: ZY
authors.lastname: Wang
authors.affiliation: Department of Food Sciences, School of Food Science and Engineer, Harbin Institute of Technology, No. 73 Huanghe Road, Nangang District, Harbin 150090, Heilongjiang Province, PR China.
authors.forename: R B
authors.initials: RB
authors.lastname: Xu
authors.affiliation: Department of Food Sciences, School of Food Science and Engineer, Harbin Institute of Technology, No. 73 Huanghe Road, Nangang District, Harbin 150090, Heilongjiang Province, PR China.
authors.forename: W J
authors.initials: WJ
authors.lastname: Li
authors.affiliation: Department of Food Sciences, School of Food Science and Engineer, Harbin Institute of Technology, No. 73 Huanghe Road, Nangang District, Harbin 150090, Heilongjiang Province, PR China.
authors.forename: Y C
authors.initials: YC
authors.lastname: Zhang
authors.affiliation: Department of Food Sciences, School of Food Science and Engineer, Harbin Institute of Technology, No. 73 Huanghe Road, Nangang District, Harbin 150090, Heilongjiang Province, PR China.
authors.forename: H
authors.initials: H
authors.lastname: Zhang
authors.affiliation: Department of Food Sciences, School of Food Science and Engineer, Harbin Institute of Technology, No. 73 Huanghe Road, Nangang District, Harbin 150090, Heilongjiang Province, PR China.
authors.forename: J
authors.initials: J
authors.lastname: Jing
mesh_terms: D000097:Acetonitriles / Q000032:analysis; D018554:Avena / Q000737:chemistry; D002851:Chromatography, High Pressure Liquid; D002523:Edible Grain / Q000737:chemistry*; D007306:Insecticides / Q000032:analysis*; D059627:Liquid Phase Microextraction; D012275:Oryza / Q000737:chemistry; D008897:Panicum / Q000737:chemistry; D010573:Pesticide Residues / Q000032:analysis*; D052616:Solid Phase Extraction; D012997:Solvents / Q000737:chemistry; D003313:Zea mays / Q000737:chemistry
chemical_list: D000097:Acetonitriles; D007306:Insecticides; D010573:Pesticide Residues; D012997:Solvents; C032159:acetonitrile