Optimization of multi-residue method for targeted screening and quantitation of 243 pesticide residues in cardamom (Elettaria cardamomum) by gas chromatography tandem mass spectrometry (GC-MS/MS) analysis

• Published in: Chemosphere (Oxford) 2018-02, Vol.193, p.447-453
• Main Authors: Ahammed Shabeer, T.P., Girame, Rushali, Utture, Sagar, Oulkar, Dasharath, Banerjee, Kaushik, Ajay, D., Arimboor, Ranjith, Menon, K.R.K.
• Format: Article
• Language: English
• Subjects: Acetates; Cardamom; Elettaria - chemistry; Gas Chromatography-Mass Spectrometry - methods; GC-MS/MS; High-Throughput Screening Assays - methods; Multi-residue method; Pesticide residues; Pesticide Residues - analysis; Pesticides - analysis; QuEChERS; Spices; Tandem Mass Spectrometry - methods
• ISSN: 0045-6535; 1879-1298
• DOI: 10.1016/j.chemosphere.2017.10.133

Higher matrix interference makes the multi-residue pesticide analysis in spices more challenging. A simple, sensitive, and robust large-scale multi-residue method was developed for the rapid analysis of 243 pesticides in cardamom matrix by gas chromatography tandem mass spectrometry (GC-MS/MS). Prehydration of cardamom in 1:4 sample:water for 30 min improved the homogeneity and extractability. QuEChERS extraction followed by cleanup with 25 mg primary secondary amine, 100 mg C18, and 10 mg graphitized carbon black to 1 ml supernatant was used for sample preparation. Reconstitution of final extract in ethyl acetate reduced matrix co-extract up to 60%. The method was validated according to the SANTE/11,945/2015 guidelines. The limit of quantification was ≤0.01 mg kg−1, and the recovery was within 70.0–120.0%, with ≤20% RSD for the majority of pesticides. The method was used for screening market samples, and the detected residues were devoid of any risk of acute toxicity related to dietary exposure. [Display omitted] •A comprehensive multi-residue GC-MS/MS method for 243 pesticides in cardamom is reported for the first time.•Solvent exchange into ethyl acetate reduces the matrix co-extractives and improves sensitivity.•The method facilitates quantification at 0.01 mg kg−1 for >78% of the target analytes in cardamom matrix.•The method was successfully applied to screen market samples.