title: Multiresidue determination of 375 organic contaminants including pesticides, polychlorinated biphenyls and polyaromatic hydrocarbons in fruits and vegetables by gas chromatography-triple quadrupole mass spectrometry with introduction of semi-quantification approach.
abstract: A residue analysis method for the simultaneous estimation of 349 pesticides, 11 PCBs and 15 PAHs extracted from grape, pomegranate, okra, tomato and onion matrices, was established by using a gas chromatograph coupled to an electron impact ionization triple quadrupole mass spectrometer (GC-EI-MS/MS). The samples were extracted by ethyl acetate and cleaned by dispersive solid phase extraction with PSA and/or GCB/C(18) by the methods reported earlier. The GC-EI-MS/MS parameters were optimized for analysis of all the 375 compounds within a 40 min run time with limit of quantification for most of the compounds at <10 μg/L, which is well below their respective European Union-Maximum Residue Levels. The coefficient of determination (r(2)) was >0.99 within the calibration linearity range of <5-250 ng/mL for compounds with LOQs<5 ng/mL. While for the compounds with LOQs within 5-10 μg/kg, the lowest calibration level was 5 and 10 μg/kg as applicable. The recoveries at 10, 25 and 50 ng/mL were within 70-110% (n=6) with associated RSDs<20% indicating satisfactory precision. The information generated from the single laboratory validation was further utilized for building a semi-quantitative approach. The accuracies in quantification obtained via individual calibration standards vis-à-vis semi-quantification approach were comparable. For incurred samples, the concentrations estimated by the semi-quantification approach were within ±10% of the values obtained by direct quantification. This approach complements the existing GC-EI-MS/MS methods by offering targeted screening and quantification capabilities.
authors.affiliation: National Referral Laboratory, National Research Centre for Grapes, P.O. Manjri Farm, Pune 412307, India. kbgrape@yahoo.com
authors.forename: Kaushik
authors.initials: K
authors.lastname: Banerjee
authors.forename: Sagar
authors.initials: S
authors.lastname: Utture
authors.forename: Soma
authors.initials: S
authors.lastname: Dasgupta
authors.forename: Chandrasekar
authors.initials: C
authors.lastname: Kandaswamy
authors.forename: Saswati
authors.initials: S
authors.lastname: Pradhan
authors.forename: Sunil
authors.initials: S
authors.lastname: Kulkarni
authors.forename: Pandurang
authors.initials: P
authors.lastname: Adsule
mesh_terms: D000085:Acetates / Q000737:chemistry; D005638:Fruit / Q000737:chemistry*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D010573:Pesticide Residues / Q000032:analysis* / Q000737:chemistry; D011078:Polychlorinated Biphenyls / Q000032:analysis* / Q000737:chemistry; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D014675:Vegetables / Q000737:chemistry*
chemical_list: D000085:Acetates; D010573:Pesticide Residues; C007650:ethyl acetate; D011078:Polychlorinated Biphenyls