title: Optimization of a sample preparation method for multiresidue analysis of pesticides in tobacco by single and multi-dimensional gas chromatography-mass spectrometry.
abstract: A selective and sensitive multiresidue analysis method, comprising 4 7pesticides, was developed and validated in tobacco matrix. The optimized sample preparation procedure in combination with gas chromatography mass spectrometry in selected-ion-monitoring (GC-MS/SIM) mode offered limits of detection (LOD) and quantification (LOQ) in the range of 3-5 and 7.5-15ng/g, respectively, with recoveries between 70 and 119% at 50-100ng/g fortifications. In comparison to the modified QuEChERS (Quick-Easy-Cheap-Effective-Rugged-Safe method: 2g tobacco+10ml water+10ml acetonitrile, 30min vortexing, followed by dispersive solid phase extraction cleanup), the method performed better in minimizing matrix co-extractives e.g. nicotine and megastigmatrienone. Ambiguity in analysis due to co-elution of target analytes (e.g. transfluthrin-heptachlor) and with matrix co-extractives (e.g. δ-HCH-neophytadiene, 2,4-DDE-linolenic acid) could be resolved by selective multi-dimensional (MD)GC heart-cuts. The method holds promise in routine analysis owing to noticeable efficiency of 27 samples/person/day.
authors.affiliation: National Referral Laboratory, National Research Centre for Grapes, P.O. Manjri Farm, Pune 412 307, India.
authors.forename: Zareen S
authors.initials: ZS
authors.lastname: Khan
authors.affiliation: Central Tobacco Research Institute, Rajahmundry, Andhra Pradesh 533105, India.
authors.forename: Rakesh Kumar
authors.initials: RK
authors.lastname: Ghosh
authors.affiliation: National Referral Laboratory, National Research Centre for Grapes, P.O. Manjri Farm, Pune 412 307, India.
authors.forename: Rushali
authors.initials: R
authors.lastname: Girame
authors.affiliation: National Referral Laboratory, National Research Centre for Grapes, P.O. Manjri Farm, Pune 412 307, India.
authors.forename: Sagar C
authors.initials: SC
authors.lastname: Utture
authors.affiliation: National Referral Laboratory, National Research Centre for Grapes, P.O. Manjri Farm, Pune 412 307, India.
authors.forename: Manasi
authors.initials: M
authors.lastname: Gadgil
authors.affiliation: National Referral Laboratory, National Research Centre for Grapes, P.O. Manjri Farm, Pune 412 307, India. Electronic address: kbgrape@yahoo.com.
authors.forename: Kaushik
authors.initials: K
authors.lastname: Banerjee
authors.affiliation: Central Tobacco Research Institute, Rajahmundry, Andhra Pradesh 533105, India.
authors.forename: D Damodar
authors.initials: DD
authors.lastname: Reddy
authors.affiliation: Central Tobacco Research Institute, Rajahmundry, Andhra Pradesh 533105, India.
authors.forename: Nalli
authors.initials: N
authors.lastname: Johnson
mesh_terms: D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D010575:Pesticides / Q000032:analysis*; D052616:Solid Phase Extraction / Q000379:methods; D012997:Solvents / Q000737:chemistry; D014026:Nicotiana / Q000737:chemistry*
chemical_list: D010575:Pesticides; D012997:Solvents
keywords: GC-MS; MDGC-MS; Matrix effect; Multiresidue analysis of pesticides; Tobacco