title: Development, validation, and uncertainty measurement of multi-residue analysis of organochlorine and organophosphorus pesticides using pressurized liquid extraction and dispersive-SPE techniques.
abstract: Simple and efficient multi-residue analytical methods were developed and validated for the determination of 13 organochlorine and 17 organophosphorous pesticides from soil, spinach and eggplant. Techniques namely accelerated solvent extraction and dispersive SPE were used for sample preparations. The recovery studies were carried out by spiking the samples at three concentration levels (1 limit of quantification (LOQ), 5 LOQ, and 10 LOQ). The methods were subjected to a thorough validation procedure. The mean recovery for soil, spinach and eggplant were in the range of 70-120% with median CV (%) below 10%. The total uncertainty was evaluated taking four main independent sources viz., weighing, purity of the standard, GC calibration curve and repeatability under consideration. The expanded uncertainty was well below 10% for most of the pesticides and the rest fell in the range of 10-20%.
authors.affiliation: Inspectorate Division, Organisation for Prohibition of Chemical Weapons, Johan de Wittlaan 32, 2517 JR, The Hague, The Netherland. doyelisanyal@gmail.com
authors.forename: Doyeli
authors.initials: D
authors.lastname: Sanyal
authors.forename: Anita
authors.initials: A
authors.lastname: Rani
authors.forename: Samsul
authors.initials: S
authors.lastname: Alam
authors.forename: Seema
authors.initials: S
authors.lastname: Gujral
authors.forename: Ruchi
authors.initials: R
authors.lastname: Gupta
mesh_terms: D004784:Environmental Monitoring / Q000379:methods; D006843:Hydrocarbons, Chlorinated / Q000032:analysis* / Q000737:chemistry; D009943:Organophosphorus Compounds / Q000032:analysis* / Q000737:chemistry; D010573:Pesticide Residues / Q000032:analysis* / Q000737:chemistry; D012987:Soil / Q000737:chemistry; D012989:Soil Pollutants / Q000032:analysis* / Q000737:chemistry; D052616:Solid Phase Extraction / Q000379:methods; D014675:Vegetables / Q000737:chemistry
chemical_list: D006843:Hydrocarbons, Chlorinated; D009943:Organophosphorus Compounds; D010573:Pesticide Residues; D012987:Soil; D012989:Soil Pollutants