title: A simple and sensitive single-step method for gas chromatography-mass spectrometric determination of fipronil and its metabolites in sugarcane juice, jaggery and sugar.
abstract: A simple and sensitive single-step method for gas chromatography-mass spectrometric determination of fipronil and its metabolites viz., fipronil desulfinyl, fipronil sulphide and fipronil sulphone in sugarcane juice, jaggery and sugar has been developed. Acetonitrile was superior to ethyl acetate in terms of selectivity, though they were on par with each other in terms of recoveries. This method does not require any cleanup as the PSA-based cleanup was on par with no-cleanup treatment. Interestingly, the recoveries of fipronil and its metabolites decreased with increased amounts of C18 from 10 to 50mg/g of matrix. Matrix effects were insignificant and the limit of quantification was 0.005μg/g. The recoveries of fipronil and its metabolites varied between 87.5% and 108.5% with the RSD of 0.2-5.3% for all the three matrices studied. This method has also been validated by monitoring fipronil and its metabolites in the retail outlet samples of sugarcane juice, jaggery and sugar.
authors.affiliation: Division of Crop Protection, Sugarcane Breeding Institute, Indian Council of Agricultural Research, Coimbatore 641007, Tamil Nadu, India. Electronic address: tramasubbu@gmail.com.
authors.forename: Thirumalaiandi
authors.initials: T
authors.lastname: Ramasubramanian
authors.affiliation: Pesticide Toxicology Laboratory, Department of Agricultural Entomology, Tamil Nadu Agricultural University, Coimbatore 641003, Tamil Nadu, India.
authors.forename: Mariappan
authors.initials: M
authors.lastname: Paramasivam
authors.affiliation: Division of Crop Protection, Sugarcane Breeding Institute, Indian Council of Agricultural Research, Coimbatore 641007, Tamil Nadu, India.
authors.forename: Ramabhadran
authors.initials: R
authors.lastname: Jayanthi
authors.affiliation: Pesticide Toxicology Laboratory, Department of Agricultural Entomology, Tamil Nadu Agricultural University, Coimbatore 641003, Tamil Nadu, India.
authors.forename: Subramaniam
authors.initials: S
authors.lastname: Chandrasekaran
mesh_terms: D002241:Carbohydrates / Q000737:chemistry*; D005591:Chemical Fractionation / Q000379:methods*; D005506:Food Contamination; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods; D007306:Insecticides / Q000032:analysis* / Q000302:isolation & purification* / Q000378:metabolism; D010936:Plant Extracts / Q000737:chemistry*; D011720:Pyrazoles / Q000032:analysis* / Q000302:isolation & purification* / Q000378:metabolism; D031786:Saccharum / Q000737:chemistry* / Q000378:metabolism
chemical_list: D002241:Carbohydrates; C060188:Gur; D007306:Insecticides; D010936:Plant Extracts; D011720:Pyrazoles; C082360:fipronil
keywords: Fipronil; Jaggery; Metabolites; Residue; Sugar; Sugarcane juice