title: Optimization of gas chromatography-single quadrupole mass spectrometry conditions for multiresidue analysis of pesticides in grapes in compliance to EU-MRLs.
abstract: A single quadrupole GC-MS method was optimized for multiresidue determination of 47 pesticides in grapes with limit of quantifications of each compound in compliance with the EU-MRL requirements. Sample preparation involved extraction of 10 g sample with 10 ml ethyl acetate (+10 g sodium sulphate) by homogenization at 15,000 rpm followed by centrifugation at 3000 rpm. The supernatant was cleaned by dispersive solid phase extraction with primary secondary amine and acidified with 0.1% formic acid. Residues were estimated in selected ion monitoring mode with programmable temperature vaporizer-large volume injection (8 μl). All the GC and MS parameters were thoroughly optimized to achieve satisfactory linearity (R(2)>0.99) within 0.01-0.25 mg kg(-1) with minimum matrix interferences. Recoveries at 0.01 and 0.02 mg kg(-1) were within 67-120% with associated precision RSD below 19%. The method was successfully applied for analysis of the real world samples for incurred residues.
authors.affiliation: National Referral Laboratory, National Research Centre for Grapes, P.O. Manjri Farm, Pune 412 307, India. kbgrape@yahoo.com
authors.forename: Kaushik
authors.initials: K
authors.lastname: Banerjee
authors.forename: Sumaiyya
authors.initials: S
authors.lastname: Mujawar
authors.forename: Sagar C
authors.initials: SC
authors.lastname: Utture
authors.forename: Soma
authors.initials: S
authors.lastname: Dasgupta
authors.forename: Pandurang G
authors.initials: PG
authors.lastname: Adsule
mesh_terms: D005062:European Union; D005506:Food Contamination / Q000032:analysis*; D059022:Food Safety; D005638:Fruit / Q000737:chemistry; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D007194:India; D010573:Pesticide Residues / Q000737:chemistry*; D027843:Vitis / Q000737:chemistry*
chemical_list: D010573:Pesticide Residues