Czech J. Food Sci., 2004, 22(5):182-189 | DOI: 10.17221/3422-CJFS

Determination of free and bound 3-chloropropane-1,2-diol by gas chromatography with mass spectrometric detection using deuterated 3-chloropropane-1,2-diol as internal standard

V. Divinová, B. Svejkovská, M. Doležal, J. Velíšek

Department of Food Chemistry and Analysis, Faculty of Food and Biotechnological Technology, Institute of Chemical Technology in Prague, Prague, Czech Republic

An improved routine, simple and sensitive method is presented for the determination of free and bound 3-chloropropane-1,2-diol (3-MCPD) in different foods using capillary gas chromatography with mass spectrometric detection and deuterated 3-MCPD as internal standard. The optimised method was linear within the working calibration standard concentrations in the range of 0.009-1.3 mg 3-MCPD per 1 kg of sample. The LOD and LOQ were 0.003 µg/kg and 0.009 µg/kg, respectively. Validation of the method was carried out by analysing standards of 3-MCPD, acid-HVP, roasted coffee samples, and the same samples spiked with 3-MCPD. Repeatability (expressed as RSD) of the method was in the range 1.0-4.2%, the average spike recoveries were 99.1-99.5% (RSD = 0.8-1.4%), respectively. 3-MCPD bound in esters with higher fatty acids was isolated as fat, the isolated fat was subjected to methanolysis and 3-MCPD generated was quantified using the same method. The LOD and LOQ were determined to be 1.1 mg/kg of lipids and 3.3 mg/kg of lipids, respectively. Using the optimised method, 20 samples of retail food products were analysed for their free and bound 3-MCPD. All samples contained free 3-MCPD at 9.6-83 µg/kg (RSD = 0.4-7.0%). The level of the bound 3-MCPD varied between the LOD and 2.4 mg/kg with RSD = 0.3-2.4%.

Keywords: 3-chloropropane-1,2-diol (3-MCPD); chloropropanediols; 3-MCPD esters; phenylboronic acid; food analysis

Published: October 31, 2004  Show citation