GAS CHROMATOGRAPHIC DETERMINATION OF 23 ORGANOPHOSPHORUS PESTICIDES RESIDUE IN BOTTLE GUARD MATRIX
Keywords:Bottle guard, Pesticides, LOD, LOQ, MRL, QuEChERS
Objective: To validate in-house QuEChERS method, which scrutinizes and quantify the residue levels of some most frequently used organophosphorus pesticides and to prove a complete workflow for routine multi-residue pesticide analysis in representative bottle guard matrices and study the persistence of 23 organ phosphorus pesticides.
Methods: QuEChERS (quick, easy, cheap, effective, rugged and safe) extraction method was followed. Method validation and residue screening of bottle guard samples were conducted by GC-FPD (Gas Chromatography-Flame Photometric Detector) were used to analyse the presence of pesticides whereas confirmation of pesticides was done by GC-MS (Gas Chromatographic-Mass Spectrometer).
Results: For bottle guard matrix, LOD (limit of detection) and LOQ (limit of quantification) values are lowest for phorate (0.005 mg/kg and 0.015 mg/kg) and highest for parathion-methyl (0.1 mg/kg and 0.3 mg/kg) respectively. Calibration curve, was plotted between an area of 23 pesticide standard mixture against seven different concentration levels of 0.01, 0.02, 0.05, 0.10, 0.20, 0.50, 1.00 mg/kg with regression coefficient (R2) are in the range of 0.978-0.994. The mean recovered amount at 0.05 mg/kg spikeing concentration are in the range of lowest 0.0413 mg/kg to highest 0.0467 mg/kg and relative standard deviation are in the range of lowest 2.2 to highest 8.571.
Conclusion: For ensuring exposure to contaminants, especially by dietary intake, Robust analytical methods were validated for carrying out both research and monitoring programmes and thus for defining limitations and supporting enforcement of regulations.
Planas C, Caixach J, Santos FJ, Rivera J. Occurrence of pesticides in spanish surface waters. Analysis by high-resolution gas chromatography coupled to mass spectrometry. Chemosphere 1997;34:2393-406.
Huber A, Bach M, Frede HG. Pollution of surface waters with pesticides in germany: modeling non-point source inputs. Agric Ecosyst Environ 2000;80:191-204.
Kidd KA, Bootsma HA, Hesslein RH. Biomagnification of DDT through the benthic and pelagic food webs of Lake Malawi, East Africa: Importance of trophic level and carbon source. Environ Sci Technol 2001;35:14-20.
Ntow WJ. Organochlorine pesticides in water, sediment, crops and human fluids in a farming community in Ghana. Arch Environ Contam Toxicol 2001;40:557-63.
Cerejeira MJ, Viana P, Batista S, Pereira T, Silva E, Valerio MJ, et al. Pesticides in portuguese surface and ground waters. Water Res 2003;37:1055-63.
Aardema H, Meertens J, Ligtenberg JJM, Peters-Polman OM, Tulleken JE, Zijlstra JG. Organophosphorus pesticide poisoning: cases and developments. Neth J Med 2008;66:149â€“53.
Lyton WB, Donald LF, Seiber NJ, Thomas RP. Ambient air concentration of pesticide in california. Environ Sci Technol 1996;30:1365â€“8.
Subhani A, Liano M, Huang CY, Xie ZM. Impact of some agronomics practices on paddy field soil health under the varied ecological condition: influence of soil moisture. Pedosphere 2001;11:38â€“48.
Toan VD, Thao VD, Walder J, Schmutz HR, Ha CT. Contamination by selected organochlorine pesticide (OCPs) in surface soil in Hanoi, Vietnam. Bull Environ Contamination Toxicol 2007;78:195â€“200.
Clothianidinâ€“Registration Status and Related Information. U. S. EPA; 2012.
PAN (Pesticide Action Network). Organophosphate Insecticides Fact Sheet. United Kingdom; 2003.
Torres CM, Pico Y, Manes J. Determination of pesticide residues in fruit and vegetablesâ€“a review. J Chromatogr 1996;754:301-31.
Durovic R, Markovic M, Markovic D. Headspace solid phase microextraction in the analysis of pesticide residuesâ€“kinetics and quantification prior to the attainment of partition equilibrium. J Serbian Chem Soc 2007a;72:879-87.
Luo L, Shao B, Zhang J. Pressurized liquid extraction and cleanup procedure for the determination of pyrethroids in soils using gas chromatography/tandem mass spectrometry. Anal Sci 2010;26:461-5.
Di Muccio A, Fidente P, Attard Barbini D, Dommarco R, Seccia S, Morrica P. Application of solid-phase extraction and liquid chromatography-mass spectrometry to the determination of neonicotinoid pesticide residues in fruit and vegetables. J Chromatogr A 2006;1108:1-6.
Lambropoulou DA, Albanis TA. Methods of sample preparation for determination of pesticide residues in food matrices by chromatographyâ€“mass spectrometry-based techniques: a review. Anal Bioanal Chem 2007;389:1663-83.
Schenck FJ, Lehotay SJ, Victor V. Comparison of solid-phase extraction sorbents for cleanup in pesticide residue analysis of fresh fruits and vegetables. J Separation Sci 2002;25:883â€“90.
Pawliszyn J. Solid-phase microextractionâ€“theory and practice. Wiley-VCH, New York, USA; 1997.
Kristenson EM, Brinkman UATh, Ramos L. Recent advances in matrix solid-phase dispersion. Trends Anal Chem 2006;25:96-111.
Anastassiades M, Scherbaum E, TaÅŸdelen B, Stajnbaher D. Recent developments in QuEChERS methodology for pesticide multiresidue analysis, pesticide chemistry. Crop Protection Public Health, Environmental Safety. Edited, H Ohkawa, H Miyagawa, PW Lee. Eds. Wiley-VCH: Weinheim, Germany; 2007. P. 439.
Lehotay SJ, Hiemstra M, Van Bodegraven P, De Kok A. Validation of a fast and easy method for the determination of more than 200 pesticide residues in fruits and vegetables using gas and liquid chromatography and mass spectrometric detection. J AOAC Int 2005;88:595-600.
Reed DV, Lombardo P, Wessel JR, Burke JA, Macmohan B. The FDA pesticides monitoring programme. JAOAC Int 1987; 70:591-5.
Sheridan RS, Meola JR. Analysis of pesticide residues in fruits, vegetables, and milk by gas chromatography/tandem mass spectrometry. J AOAC Int 1999;82:982-90.
Lehotay SJ. Determination of pesticide residues in nonfatty foods by supercritical fluid extraction and gas chromatography/mass spectrometry: collaborative study. J AOAC Int 2000;83:680-97.
Anastassiades M, Mastovska K, Lehotay SJ. Evaluation of analyte protectants to improve gas chromatographic analysis of pesticides. J Chromatogr A 2003;1015:163-84.
Hernandez Borges J, Cabrera JC, Rodriguez Delgado MA, Hernandez Suarez EM, Sauco VG. Analysis of pesticide residues in bananas harvested in the Canary Islands (Spain). Food Chem 2009;113:313â€“9.
Lehotay SJ, Mastovska K, Yun SJ. Evaluation of two fast and easy methods for pesticide residue analysis in fatty food matrixes. J AOAC Int 2005;88:630-8.
Nguyen TD, Yu JE, Lee DM, Lee GH. A multiresidue method for the determination of 107 pesticides in cabbage and radish using QuEChERS sample preparation method and gas chromatography-mass spectrometry. Food Chem 2008; 110:207â€“13.
Anastasiades M, Lehotay SJ, Stajnbaher D, Schenck FJ. Fast and easy multi-residue method employing acetonitrile extraction/ partitioning and dispersive solid-phase extraction for the determination of pesticide residues in produce. J AOAC Int 2003;86:412-31.
Lehotay SJ. Determination of pesticide residues in foods by acetonitrile extraction and partitioning with magnesium sulfate: collaborative study. J AOAC Int 2007;90:485â€“520.
Srikanth I, Prameela Rani A. Development and validation of liquid chromatography coupled with tandem mass spectrometry method for estimation of Lenvatinib in human plasma. Asian J Pharm Clin Res 2017;10:120-6.
Corley J. Best practices in establishing detection and quantification limits for pesticide residues in foods. Rutgers, The State University of New Jersey, North Brunswick, NJ: USA; 2002.
Corley J. Best practices in establishing detection and quantification limits for pesticide residues in foods, Handbook of Residue Analytical Methods for Agrochemicals. Wiley and Sons. New York: USA; 2003. p. 59-74.
Sharma KK. Pesticide residue analysis Manual, Indian council of agriculture research. New Delhi; 2013. p. 218-33.
Saini MK, Mishra S, Alam S, Thakur LK, Raza SK. Method development and validation of multiclass pesticide residues and metabolites in wheat by GC-ECD and GC-MS. Asian J Res Chem 2016;9:1-9.
Mishra S, Saini MK, Alam S, Thakur LK, Raza SK. Method validation and uncertainty measurement for determination of 25 pesticides by GC-ECD and MSD in banana using modified QuEChERS technique. Int Res J Environ Sci 2015;4:21-7.
Mishra S, Saini MK, Alam S, Thakur LK, Raza SK. Determination of 25 pesticides by GC-ECD and MSD with measurement of uncertainty in tomato using modified QuEChERS technique. J Appl Chem 2015;4:221-31.