title: Development and validation of ethylenethiourea determination in foods using methanol-based extraction, solid-phase extraction cleanup and LC-MS/MS.
abstract: To response to the need for a rapid, cost-effective, eco-friendly and efficient extraction process, a sensitive method for the determination of ethylenethiourea (ETU) in food matrices by high-performance liquid chromatography-mass spectrometry (HPLC-LC/MS) was developed and validated. ETU was extracted from food commodities with methanol, cleaned up by alumina-SPE column, and then determined by HPLC-MS/MS. The MS detection was operated in positive ionization mode. For confirmation of target compound, two precursor ion>product ion transitions were selected by multi-reaction monitoring mode (MRM). The method showed good linearity with correlation coefficient higher than 0.9950. Recoveries at three spiked levels (10, 50, 100 ng/g) in random selected food matrices were in range of 71-121% with RSDs not larger than 25%. The limit of quantitation for the analyte was estimated at 5 ng/g.
authors.affiliation: Total Diet and Pesticide Research Center, US Food and Drug Administration, Office of Regulatory Affairs, 11510 W 80th St., Lenexa, KS 66214, USA. kevin.tran@fda.hhs.gov
authors.forename: Kevin
authors.initials: K
authors.lastname: Tran
authors.forename: Lucie P
authors.initials: LP
authors.lastname: Mactal
authors.forename: Michele R
authors.initials: MR
authors.lastname: Cromer
authors.forename: Ralph H
authors.initials: RH
authors.lastname: Vocque
authors.forename: Robert E
authors.initials: RE
authors.lastname: Smith
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D005031:Ethylenethiourea / Q000032:analysis* / Q000302:isolation & purification*; D005504:Food Analysis; D005506:Food Contamination / Q000032:analysis*; D005659:Fungicides, Industrial / Q000032:analysis*; D052616:Solid Phase Extraction / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D005659:Fungicides, Industrial; D005031:Ethylenethiourea