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  • Multiresidue analysis of 83 pesticides and 12 dioxin-like polychlorinated biphenyls in wine by gas chromatography-time-of-flight mass spectrometry.

Multiresidue analysis of 83 pesticides and 12 dioxin-like polychlorinated biphenyls in wine by gas chromatography-time-of-flight mass spectrometry.

Journal of chromatography. A (2009-02-14)
Sangram H Patil, Kaushik Banerjee, Soma Dasgupta, Dasharath P Oulkar, Shubhangi B Patil, Manjusha R Jadhav, Rahul H Savant, Pandurang G Adsule, Madhukar B Deshmukh
ABSTRACT

A multiresidue method is described for simultaneous estimation of 83 pesticides and 12 dioxin-like polychlorinated biphenyls (PCBs) in red and white wines. The samples (20mL wine, acidified with 20 mL 1% HCl) were extracted with 10 mL ethyl acetate (+20 g sodium sulphate) and cleaned by dispersive solid-phase extraction (DSPE) with anhydrous calcium chloride and Florisil successively. The final extract (5 mL) was solvent exchanged to 1mL of cyclohexane:ethyl acetate (9:1), further cleaned by DSPE with 25mg primary secondary amine sorbent and analyzed by gas chromatography-time-of-flight mass spectrometry (GC-TOF-MS) within 31 min run time. The limits of quantification of most analytes were <or=10-20 microg/L. Acidification of wine prior to extraction prevented hydrolysis of organophosphorous pesticides as well as dicofol, whereas treatment with CaCl(2) minimized the fatty acid co-extractives significantly. Solvent exchange to cyclohexane:ethyl acetate (9:1) further minimized the co-extractives. Recoveries at 5, 10 and 20 ng/mL were >80% for most analytes except cyprodinil, buprofezin and iprodione. The expanded uncertainties at 10 ng/mL were <20% for most analytes. Intra-laboratory precision in terms of Horwitz ratio of all the analytes was below 0.5, suggesting ruggedness of the method. Effectively, the method detection limit for most analytes was as low as up to 1 ng/mL in both red and white wine, except for cyfluthrin and cypermethrin.

MATERIALS
Product Number
Brand
Product Description

Supelco
Florisil® Adsorbent for Chromatography, 30-60 mesh
Supelco
Florisil® Adsorbent for Chromatography, 60-100 mesh
Supelco
Florisil® PR, PR grade (analysis acc. to FDA)
Sigma-Aldrich
Florisil®, 100-200 mesh
Supelco
Florisil®, 100-200 mesh, fine powder
Supelco
Florisil®, PR grade, 60-100 mesh, coarse powder
Supelco
Florisil®, <200 mesh, fine powder
Supelco
Florisil®, for the determination of hydrocarbon acc. to ISO 9377-2