BS EN 14573:2004 – Foodstuffs — Determination of 3-monochloropropane- 1,2-diol by GC/MS
1 Scope
This document specifies a gas chromatographic method using mass spectrometric detection for the determination of 3-monochloropropane-1 ,2-diol (3-MCPD) in hydrolysed vegetable proteins and other foodstuffs [1 ]. The method has been validated in interlaboratory studies for malt extract, soup powder, bread crumbs, salami sausage, cheese alternative and hydrolysed vegetable protein.
2 Principle
The sample is mixed with a deuterated internal standard, with sodium chloride solution and with a solid support material. The mixture is transferred to a chromatographic column and is first extracted with a mixture of n-hexane and diethyl ether for removing non-polar components. Then, 3-MCPD is eluted with diethyl ether, the eluate is concentrated and an aliquot portion is derivatized using heptafluorobutyrylimidazole. The solution is analyzed by gas chromatography using mass spectrometric detection [2].
3 Reagents
3.1 General
Unless otherwise specified, use reagents of recognized analytical quality and distilled or demineralized water.
Take every precaution to avoid possible contamination of water, solvents, inorganic salts etc. by plastics and rubber materials. Use only glass containers for storage and handling of all water and reagents.
WARNING — The use of this standard may involve hazardous materials, operations and equipment.
This standard does not purport to address all the safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
3.2 n-Hexane, glass distilled
3.3 Diethyl ether, glass distilled
3.4 2,2,4-Trimethylpentane
3.5 Ethyl acetate
3.6 Solvent mixture, n-hexane (3.2) and diethyl ether (3.3) 9+1 (V/V)
3.7 Sodium chloride solution, 290 g of sodium chloride dissolved in 1 l of water
3.8 Sodium sulfate, anhydrous
3.9 Heptafluorobutyrylimidazole
3.11 3-Monochloropropane-1,2-diol (3-MCPD)
3.12 d5-3-Monochloropropane-1,2-diol (d5-3-MCPD), minimum 98 % isotopic purity
The stability of d5-3-Monochloropropane-1 ,2-diol (d5-3-MCPD) is limited and should be checked .
3.13 3-MCPD stock solution, ρ (3-MCPD) = 1 mg/ml
Weigh 25 mg of 3-MCPD (3.1 1 ) and dilute to the mark with ethyl acetate (3.5) in a 25 ml volumetric flask.
3.14 3-MCPD standard solutions
Dilute 1 0 ml of the 3-MCPD stock solution (3.1 3) to the mark with ethyl acetate (3.5) in a 1 00 ml volumetric flask. From this dilution, transfer volumes of each 0 µl, 1 2,5 µl, 25 µl, 1 25 µl, 250 µl and 500 µl into 25 ml volumetric flasks and dilute to the mark with 2,2,4-trimethylpentane (3.4) to give 0 µg/ml, 0,05 µg/ml,0,1 0 µg/ml, 0,50 µg/ml, 1 ,0 µg/ml, and 2,0 µg/ml 3-MCPD.
3.15 d5-3-MCPD stock solution, ρ(d5-3-MCPD) = 1 mg/ml
Weigh 25 mg of d5-3-MCPD (3.1 2) and dilute to the mark with ethyl acetate (3.5) in a 25 ml volumetric flask.
3.16 d5-3-MCPD internal standard solution, ρ(d5-3-MCPD) = 1 0 µg/ml
Dilute 1 ,0 ml of the d5-3-MCPD stock solution (3.1 5) to the mark with ethyl acetate (3.5) in a 1 00 ml volumetric flask.
BS EN 14573:2004 – Foodstuffs — Determination of 3-monochloropropane- 1,2-diol by GC/MS