title: A novel optimised and validated method for analysis of multi-residues of pesticides in fruits and vegetables by microwave-assisted extraction (MAE)-dispersive solid-phase extraction (d-SPE)-retention time locked (RTL)-gas chromatography-mass spectrometry with Deconvolution reporting software (DRS).
abstract: A rapid, effective and ecofriendly method for sensitive screening and quantification of 72 pesticides residue in fruits and vegetables, by microwave-assisted extraction (MAE) followed by dispersive solid-phase extraction (d-SPE), retention time locked (RTL) capillary gas-chromatographic separation in trace ion mode mass spectrometric determination has been validated as per ISO/IEC: 17025:2005. Identification and reporting with total and extracted ion chromatograms were facilitated to a great extent by Deconvolution reporting software (DRS). For all compounds LOD were 0.002-0.02mg/kg and LOQ were 0.025-0.100mg/kg. Correlation coefficients of the calibration curves in the range of 0.025-0.50mg/kg were >0.993. To validate matrix effects repeatability, reproducibility, recovery and overall uncertainty were calculated for the 35 matrices at 0.025, 0.050 and 0.100mg/kg. Recovery ranged between 72% and 114% with RSD of <20% for repeatability and intermediate precision. The reproducibility of the method was evaluated by an inter laboratory participation and Z score obtained within ±2.
authors.affiliation: University School of Basic and Applied Sciences, GGS Indraprastha University, Kashmere Gate, Delhi 110403, India.
authors.forename: Gouri
authors.initials: G
authors.lastname: Satpathy
authors.affiliation: University School of Basic and Applied Sciences, GGS Indraprastha University, Kashmere Gate, Delhi 110403, India. Electronic address: drytyagi@gmail.com.
authors.forename: Yogesh Kumar
authors.initials: YK
authors.lastname: Tyagi
authors.affiliation: University School of Biotechnology, GGS Indraprastha University, Kashmere Gate, Delhi 110403, India.
authors.forename: Rajinder Kumar
authors.initials: RK
authors.lastname: Gupta
keywords: Dispersive solid-phase extraction (d-SPE); Fruits and vegetables; Gas chromatography–mass spectrometry; Method validation; Microwave-assisted extraction (MAE); Pesticides