The results of the assessment of the dietary exposure to annatto, nitrites, tartaric acid and sulphites within the framework of the second French total diet study (TDS) are reported. These 4 additives were selected from the Bemrah et al. study [Bemrah N, Leblanc JC, Volatier JL. 2008. Assessment of dietary exposure in the French population to 13 selected food colours, preservatives, antioxidants, stabilizers, emulsifiers and sweeteners. Food Addit Contam B. 1(1):2-14] on 13 food additives which identified a possible health risk for annatto, sulphites and nitrites and a lack of data for tartaric acid. Among the composite samples selected for the whole TDS, 524 were analysed for additives (a sample was analysed for a given additive when it was identified as a major contributor for this additive only): 130 for tartaric acid, 135 for nitrites, 59 for annatto and 200 for sulphites. Estimated concentrations (minimum lower bound to maximum upper bound) vary nationally from 0 to 9 mg/kg for annatto, 0 to 420 mg/kg for tartaric acid, 0 to 108 mg/kg for sulphites and 0 to 3.4 mg/kg for nitrites. Based on the analytical results, the dietary exposure was calculated for adults and children, separately, using lower bound and upper bound assumptions. The European ADIs for these 4 additives were not exceeded except for the dietary exposure for sulphites among 2.9% of the adult population, where the major contributors were alcoholic drinks and especially wine under both hypotheses (lower and upper bound).
This paper reports the application of a GC/MS method for the quantification of 3-chloropropane-1,2-diol (3-MCPD) at low microg kg-1 levels through the determination of its 1,3-dioxolane derivative to a wide range of foodstuffs. The proposed protocol is based on the methods generally performed in control laboratories. The two main stages of the method - the solid-phase extraction and the purification of the derivatives - have been optimized. The within-laboratory reproducibility meets the official performance criteria for verifying 3-MCPD at the 20 microg kg(-1) limit stipulated by the European Community for soy sauce. The limit of quantification was below 5 microg kg(-1) for all the foodstuffs analysed. This method offers a valuable alternative to the draft CEN European Standard: instead of diethyl ether, much safer ethyl acetate is used; derivatization is more selective; and reagents are common stable chemicals. This method was successfully applied to toasted bread, savoury crackers, cheese, soups, including vegetable-based soups, meat products such as salami, vegetable oils, sauces, soy sauce and related products. Upon checking the method performance in the case of vegetable oils, the unexpected presence of monobromopropanediols was detected.
This paper describes a method for the determination of 3-monochloropropane-1,2-diol and 2-monochloropropane-1,3-diol (MCPD) esters and glycidyl esters in various foodstuffs, which are isolated using microwave extraction. The next step is based on alkaline-catalyzed ester cleavage. The released glycidol is transformed into monobromopropanediol (MBPD). All compounds are derivatized in free diols (MCPD and MBPD) with phenylboronic acid and analyzed by gas chromatography-mass spectrometry (GC-MS). The method was validated for oils with a limit of quantitation (LOQ) of 0.1 mg/kg, for chips and crisps with a LOQ of 0.02 mg/kg, and for infant formula with a LOQ of 0.0025 mg/L. Recoveries of each sample were controlled by standard addition on extracts before derivatization. Quantitation was performed by the addition of isotopically labeled glycidyl and 3-monochloropropane-1,2-diol (3-MCPD) esters.
A method for the determination of ethylendiaminetetraacetic acid (EDTA) in foodstuffs by high performance liquid chromatography (HPLC) and gas chromatography (GC) is described. This method is applied to foodstuffs rich in sugars and polysaccharides for which aqueous extraction cannot be directly used in chromatographic analysis. EDTA, in its iron chelate form, is extracted with water from the defatted foodstuff. The extract is then purified by ion-exchange chromatography. At this stage of purification, the quantitative level of EDTA can be estimated by HPLC and the result can be confirmed by GC. The detection level of our samples of tinned beans was under 5 mg/kg.
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