title: Validation of a QuEChERS-based gas chromatographic method for analysis of pesticide residues in Cassia angustifolia (senna).
abstract: A simple multi-residue method based on modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) approach was established for the determination of 17 organochlorine (OC), 15 organophosphorous (OP) and 7 synthetic pyrethroid (SP) pesticides in an economically important medicinal plant of India, Senna (Cassia angustifolia), by gas chromatography coupled to electron capture and flame thermionic detectors (GC/ECD/FTD) and confirmation of residues was done on gas chromatograph coupled with mass spectrometry (GC-MS). The developed method was validated by testing the following parameters: linearity, limit of detection (LOD), limit of quantification (LOQ), matrix effect, accuracy-precision and measurement uncertainty; the validation study clearly demonstrated the suitability of the method for its intended application. All pesticides showed good linearity in the range 0.01-1.0 μg mL(-1) for OCs and OPs and 0.05-2.5 μg mL(-1) for SPs with correlation coefficients higher than 0.98. The method gave good recoveries for most of the pesticides (70-120%) with intra-day and inter-day precision < 20% in most of the cases. The limits of detection varied from 0.003 to 0.03 mg kg(-1), and the LOQs were determined as 0.01-0.049 mg kg(-1). The expanded uncertainties were <30%, which was distinctively less than a maximum default value of ±50%. The proposed method was successfully applied to determine pesticide residues in 12 commercial market samples obtained from different locations in India.
authors.affiliation: a ICAR-Directorate of Medicinal and Aromatic Plants Research , Anand , Gujarat , India.
authors.forename: Vandana
authors.initials: V
authors.lastname: Tripathy
authors.affiliation: a ICAR-Directorate of Medicinal and Aromatic Plants Research , Anand , Gujarat , India.
authors.forename: Ajoy
authors.initials: A
authors.lastname: Saha
authors.affiliation: b Pesticide Residue Laboratory, Anand Agricultural University , Anand , Gujarat , India.
authors.forename: Dilipkumar J
authors.initials: DJ
authors.lastname: Patel
authors.affiliation: a ICAR-Directorate of Medicinal and Aromatic Plants Research , Anand , Gujarat , India.
authors.forename: B B
authors.initials: BB
authors.lastname: Basak
authors.affiliation: b Pesticide Residue Laboratory, Anand Agricultural University , Anand , Gujarat , India.
authors.forename: Paresh G
authors.initials: PG
authors.lastname: Shah
authors.affiliation: a ICAR-Directorate of Medicinal and Aromatic Plants Research , Anand , Gujarat , India.
authors.forename: Jitendra
authors.initials: J
authors.lastname: Kumar
mesh_terms: D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D007194:India; D057230:Limit of Detection; D013058:Mass Spectrometry; D010573:Pesticide Residues / Q000032:analysis*; D010575:Pesticides / Q000032:analysis*; D012676:Senna Extract / Q000032:analysis*; D029846:Senna Plant / Q000737:chemistry*
chemical_list: D010573:Pesticide Residues; D010575:Pesticides; D012676:Senna Extract
keywords: Gas chromatograph; QuEChERS; organochlorine; organophosphorus; pesticides residues; senna