title: Simultaneous determination of 346 multiresidue pesticides in grapes by PSA-MSPD and GC-MS-SIM.
abstract: The article demonstrates a method of simultaneous determination for 352 pesticide residues in grapes using primary-secondary amine (PSA) matrix solid phase dispersion (MSPD) cleanup and gas chromatography-mass spectrometry-selected ion monitoring (GC-MS-SIM). Grape samples (15 g) were mixed with 6 g of anhydrous magnesium sulfate and 1.5 g of sodium chloride, and then extracted with acetonitrile (15 mL) and cleaned up with 0.3 g of dispersive PSA. The analytes were determined by GC-MS-SIM. Four injections for one sample were acquired to cover a total of 352 pesticides. The limit of detection (LOD) for the method was 0.0017-0.2667 mg kg(-1), depending on the nature of compounds. The linear correlation coefficient (r) was equal to or greater than 0.95; at low, medium, and high fortification levels, recoveries ranged from 45% to 136% for 352 pesticides, among which the recoveries between 60%-120% accounted for 97%. The pesticides for which the relative standard deviations (RSD) were equal to or below 20% accounted for 95%. A positive of nine varieties of grape samples was detected out, one of which was abtained Changli city, Hebei province, China. Pesticides were identified by the retention time, molecule ions, fragment ions, and the abundance ratio of the selected ions. The analytical method was rugged, quick, cheap and effective, and suitable for the determination of a wide scope of 346 pesticides in grapes.
authors: Shandong Agricultural University, 61 Daizong Street, Taian, Shandong 271018, China.
authors: Yu-Jing
authors: YJ
authors: Lian
authors: Guo-Fang
authors: GF
authors: Pang
authors: Huai-Rui
authors: HR
authors: Shu
authors: Chun-Lin
authors: CL
authors: Fan
authors: Yong-Ming
authors: YM
authors: Liu
authors: Jie
authors: J
authors: Feng
authors: Yan-Ping
authors: YP
authors: Wu
authors: Qiao-Ying
authors: QY
authors: Chang
mesh_terms: D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D057230:Limit of Detection; D010573:Pesticide Residues / Q000032:analysis*; D015203:Reproducibility of Results; D027843:Vitis / Q000737:chemistry*
chemical_list: D010573:Pesticide Residues