Validation of a QuEChERS-based gas chromatographic method for analysis of pesticide residues in Cassia angustifolia (senna)

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 Ind...

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Published in:Journal of environmental science and health. Part B, Pesticides, food contaminants, and agricultural wastes Pesticides, food contaminants, and agricultural wastes, 2016-08, Vol.51 (8), p.508-518
Main Authors: Tripathy, Vandana, Saha, Ajoy, Patel, Dilipkumar J., Basak, B. B., Shah, Paresh G., Kumar, Jitendra
Format: Article
Language:English
Subjects:
Cassia angustifolia
Chromatography
Gas chromatograph
Gas Chromatography-Mass Spectrometry - methods
India
Limit of Detection
Mass Spectrometry
organochlorine
organophosphorus
Pesticide Residues - analysis
Pesticides
Pesticides - analysis
pesticides residues
QuEChERS
senna
Senna Extract - analysis
Senna Plant - chemistry
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Summary: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
ISSN:0360-1234
1532-4109
DOI:10.1080/03601234.2016.1170544