Determination of the Chloropropanols, 3-Chloro-1,2-propandiol and 2-Chloro-1,3-propandiol, in Hydrolysed Vegetable Proteins and Seasonings by Gas Chromatography/Ion Trap Tandem Mass Spectrometry

Abstract

This paper reports on the development of a highly selective method for the determination of parts-per-billion (µg/kg) levels of 3-chloro-1,2-propandiol (3-MCPD) in hydrolysed vegetable proteins (HVP) using gas chromatography/ion trap mass spectrometry operating in the tandem mass spectrometry (MS/MS) mode. Samples were extracted into 5M sodium chloride solution and partitioned into diethyl ether using Extrelut® 20 solid phase columns. Dried and concentrated extracts were derivatized with heptafluorobutyrylimidazole (HFBI) prior to determination by gas chromatography ion trap (GC/IT) MS/MS. Multiple reaction monitoring was used to monitor the parent/daughter ion transitions of the analytes and the stable isotope internal standard (3-chloro-1,2-propandiol-d 7 ). Calibration was linear over the range 5.0-500 pg/µL with correlation coefficients of 0.999 routinely obtained. The results showed that the method was capable of detecting 3-MCPD below 5 µg/kg in HVP when analysed by GC/ITMS/MS.

Determination of 3-chloropropane-1,2-diol as its 1,3-dioxolane derivative at the μg kg−1level: Application to a wide range of foods

“…Diethyl ether is the solvent most commonly used to elute 3-MCPD (Hamlet and Sutton 1997;Meierhans et al 1998;Macarthur et al 2000;Crews et al 2002;Hamlet et al 2002b). It has been selected as the extraction solvent for the draft European Standard.…”

“…Only those methods based on a solid-phase extraction, derivatization and GC/MS analysis of the derivative enable the quantification of 3-MCPD in foods at the mg kg À1 level. After a solid-phase extraction, generally with diethyl ether as the solvent, 3-MCPD is converted either to the diheptafluorobutyrate ester (Hamlet et al 1997(Hamlet et al , 1998Brereton et al 2001;Chung et al 2002) or to 4-chloromethyl-2, 2-dimethyl-1,3-dioxolane (Meierhans et al 1998).…”

Rapid and simple determination of chloropropanols (3-MCPD and 1,3-DCP) in food products using isotope dilution GC–MS

“…All recent methods for the determination of chloropropanols are based on gas chromatography-mass spectrometry (GC-MS). Hamlet and Sutton (1997) and Hamlet (1998) applied tandem ion trap GC-MS for the determination of 3-MCPD and 2-MCPD in soy-related products. Meierhans, Bruehlmann, Meili, and Taeschler (1998) applied Extrelut column ether extraction, derivatization with acetone and GC-MS for the determination of 3-MCPD and 2-MCPD in seasonings and soy products.…”

3‐Chloropropane‐1,2‐diol (3‐MCPD) in Soy Sauce: A Review on the Formation, Reduction, and Detection of This Potential Carcinogen

“…The LOD is between 0.01 and 0.10 mg/kg. Hamlet and Sutton () combined HFBI derivatization with GC‐MS/MS MRM and achieved a detection limit of 0.05 × 10 −1 mg/kg, which was low enough to meet the EU requirement. Robert and others () and Bel‐Rhlid and others () researched the combination of HFBI and GC‐MS, and the LOD was 0.05 × 10 −1 mg/kg.…”