Development and validation of ethylenethiourea determination in foods using methanol-based extraction, solid-phase extraction cleanup and LC-MS/MS. 2013

Kevin Tran, and Lucie P Mactal, and Michele R Cromer, and Ralph H Vocque, and Robert E Smith
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

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.

UI MeSH Term Description Entries
D002851 Chromatography, High Pressure Liquid Liquid chromatographic techniques which feature high inlet pressures, high sensitivity, and high speed. Chromatography, High Performance Liquid,Chromatography, High Speed Liquid,Chromatography, Liquid, High Pressure,HPLC,High Performance Liquid Chromatography,High-Performance Liquid Chromatography,UPLC,Ultra Performance Liquid Chromatography,Chromatography, High-Performance Liquid,High-Performance Liquid Chromatographies,Liquid Chromatography, High-Performance
D005031 Ethylenethiourea A degradation product of ethylenebis(dithiocarbamate) fungicides. It has been found to be carcinogenic and to cause THYROID hyperplasia. Imidazolidinethione,2-Mercaptoimidazoline,Imidazolidine-2-thione,2 Mercaptoimidazoline
D005504 Food Analysis Measurement and evaluation of the components of substances to be taken as FOOD. Analysis, Food,Analyses, Food,Food Analyses
D005506 Food Contamination The presence in food of harmful, unpalatable, or otherwise objectionable foreign substances, e.g. chemicals, microorganisms or diluents, before, during, or after processing or storage. Food Adulteration,Adulteration, Food,Adulterations, Food,Contamination, Food,Contaminations, Food,Food Adulterations,Food Contaminations
D005659 Fungicides, Industrial Chemicals that kill or inhibit the growth of fungi in agricultural applications, on wood, plastics, or other materials, in swimming pools, etc. Industrial Fungicides
D052616 Solid Phase Extraction An extraction method that separates analytes using a solid phase and a liquid phase. It is used for preparative sample cleanup before analysis by CHROMATOGRAPHY and other analytical methods. Extraction, Solid Phase,Extractions, Solid Phase,Solid Phase Extractions
D053719 Tandem Mass Spectrometry A mass spectrometry technique using two (MS/MS) or more mass analyzers. With two in tandem, the precursor ions are mass-selected by a first mass analyzer, and focused into a collision region where they are then fragmented into product ions which are then characterized by a second mass analyzer. A variety of techniques are used to separate the compounds, ionize them, and introduce them to the first mass analyzer. For example, for in GC-MS/MS, GAS CHROMATOGRAPHY-MASS SPECTROMETRY is involved in separating relatively small compounds by GAS CHROMATOGRAPHY prior to injecting them into an ionization chamber for the mass selection. Mass Spectrometry-Mass Spectrometry,Mass Spectrometry Mass Spectrometry,Mass Spectrometry, Tandem

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