Optimization of a sample preparation method for multiresidue analysis of pesticides in tobacco by single and multi-dimensional gas chromatography-mass spectrometry

• Published in: Journal of Chromatography A Vol. 1343; pp. 200 - 206
• Main Authors: Khan, Zareen S., Ghosh, Rakesh Kumar, Girame, Rushali, Utture, Sagar C., Gadgil, Manasi, Banerjee, Kaushik, Reddy, D. Damodar, Johnson, Nalli
• Format: Journal Article
• Language: English
• Published: Amsterdam Elsevier B.V 23.05.2014; Elsevier
• Subjects: Agrochemicals products; Biological and medical sciences; Fundamental and applied biological sciences. Psychology; Gas Chromatography-Mass Spectrometry - methods; GC-MS; Generalities; Matrix effect; MDGC-MS; Medical sciences; Multiresidue analysis of pesticides; Nicotiana - chemistry; Pesticides - analysis; Phytopathology. Animal pests. Plant and forest protection; Pollution effects and side effects of agrochemicals on crop plants and forest trees. Other anthropogenic factors; Pollution effects. Side effects of agrochemicals; Solid Phase Extraction - methods; Solvents - chemistry; Tobacco; Tobacco, tobacco smoking; Toxicology; Multiresidue analysis of pesticides; GC-MS; MDGC-MS; Tobacco; Matrix effect; Chemical analysis; Solvent extraction; Nicotiana tabacum; Multiresidue analysis; Optimization; Chemical enrichment; Dispersive Solid-Phase Extraction; Sample preparation; Dicotyledones; Angiospermae; Solanaceae; Validation; Multidimensional chromatography; Coupled method; Pesticides; Contamination; Gas chromatography; Multicomponent analysis; Residue; Spermatophyta; Mass spectrometry
• ISSN: 0021-9673; 1873-3778
• DOI: 10.1016/j.chroma.2014.03.080

•An effective multiresidue analysis method reported for 47 pesticides in tobacco.•Resolved analytes from co-eluted matrix by multi-dimensional GC heart-cut.•Analysis by GC-MS/SIM with an output of 27 samples/person/day. 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.