Appendix: method procedure summary

20 E472e: Monodiacetyl tartaric acid esters of monodiglycerides of fatty acids

20.1 Introduction

The major food groups contributing to dietary intake of monodiacetyl tartaric acid esters of monodiglycerides of fatty acids emulsifiers are desserts, pizza, meat spreads, cakes, ice-cream, bread and poultry with no maximum level of use set. It is used in accordance with good manufacturing practice to achieve the desired technological effect. The acceptable daily intake ADI for monodiacetyl tartaric acid esters of monodiglycerides of fatty acids is 50 mgkg body weight.

20.2 Methods of analysis

Very few methods are published for the determination of monodiacetyl tartaric acid esters of monodiglycerides of fatty acids in foodstuffs. The most recent publications found were those dating from the 1980s and early 1990s. An HPLC method for diacetyl tartaric acid esters in flour, 1 a GC method for diacetyl tartaric acid ester of diglyceride in coffee cream powders 2 and an HPLC method for the analysis of the emulsifiers, sodium stearoyl lactylate E481, calcium stearoyl lactylate E482 and monodiacetyl tartaric acid esters of monodiglycerides of fatty acids E472e. 3 These were for the substances themselves and not for their analysis in foods. A summary of these methods is given in Table 20.1, together with the matrices for which the methods are applicable. If statistical parameters for these methods were available these have been summarised in Table 20.2.

20.3 Recommendations

There are no recent publications for methods of analysis for monodiacetyl tartaric acid esters of monodiglycerides of fatty acids. This is therefore an area that requires method development ensuring that the methods are applicable to desserts, pizza, meat spreads, cakes, ice-cream, bread and poultry.

20.4 References

1 ‘Méthode de detection par chromatographie liquide haute pression de l’acide tartrique constitutive des émulsifiants E 472e et utilisés comme additives dans les farines’, Wirsta P, Corbel M. Industries des Céréales 1994 86, 46–51. [French] 2 ‘Gas–liquid chromatographic detection and determination of diacetyl tartaric acid esters of diglyceride in dairy and nondairy coffee cream powders’, Inoue T, Iwaida M, Ito Y, Tonogai Y. J. Assoc. Off. Anal. Chem. 1981 612, 276–279. 3 ‘Analytical and structural study of some foods emulsifiers by high-performance liquid chromatography and off-line mass spectrometry’, Sudraud G, Coustard J M, Retho C, Caude M, Rosset R, Hagemann R, Guadin D, Virelizier H. Journal of Chromatogaphy 1981 204, 397–406. E472e: Monodiacetyl tartaric acid esters of monodiglycerides 207 Table 20.1 Summary of methods for monodiacetyl tartaric acid esters of monodiglycerides of fatty acids in foods Method Matrix Sample preparation Method conditions Detection Reference IP-HPLC Flour Extraction with ethyl acetate, saponification Nucleosil C18 column at 30 ºC with UV at 200 nm 1 and acidification of the extract followed by acetonitrile:TBA–H 2 PO 4 40 mM, direct injection of a dilute aliquot pH 6.5 15:85 mobile phase at 1 mLmin and 10 µL injection GC Coffee cream Extracted under acidic conditions with ethyl Glass column 150 cm × 3 mm packed FID at 250 ºC 2 powder acetate, saponified, acidified. Free fatty acids with 1.5 silicone SE-30 on 80–100 removed with ether and reaction mixture was mesh Chromosorb G at 165 ºC, adsorbed on anion exchange column. Tartaric 5 µL injection at 250 ºC, nitrogen acid eluted with 2 N HCl–acetone1:1. Aliquot flow 20 mLmin of TMS derivative of the eluate was injected HPLC–MS Emulsifiers Complex mixtures separated by semi- The different products of the more Mass spectrometry 3 preparative adsorption liquid chromatography polar compounds were identified by using 4 separate isocratic runs using mobile off-line mass spectrometry of the phases of decreasing elution strength trimethylsilyl derivatives and the medium polar and apolar compounds were identified by their mass spectra as determined by GC–MS 208 Analytical methods for food additives Table 20.2 Summary of statistical parameters for monodiacetyl tartaric acid esters of monodiglycerides of fatty acids in foods Method Matrix Extent of validation Statistical parameters Reference GC Coffee cream Method used for coffee cream Recoveries of diacetyl tartaric acid esters of diglyceride DTDG 2 powder powder added at 50, 200, 2000 ppm levels to a coffee cream powder were 85.6–99.5 .