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E355–7, E359: Adipic acid and its salts  175


            methods need developing for the determination of adipic acid and its salts in
            desserts as this is the major food group contributing to dietary intake of adipic acid.
              A method published in 1979 for the analysis of adipic acid in orange soft drinks 1
            was carried out on a concentrated orange soft drink known and verified to be free
            of adipic acid, which was contaminated with 0.125 g adipic acid/kg in diluted
            solution (1+4). The prepared dilution was sent to 6 laboratories in Japan for
            analysis The method consisted of extraction and derivatisation before analysing
                  .
            by gas–liquid chromatography with flame ionisation detection. The procedure for
            this method is given in Appendix 1 and the performance characteristics are given
            in Table 14.3.
              An improved GC determination of adipate in starch was internationally
                               4
            collaboratively trialled.  The method is summarised in Appendix 2 and the
            performance characteristics are given in Table 14.4.


            14.3  Recommendations
            The improved GC determination of adipate in starch has been fully validated but
            there are few published methods for adipic acid in foods. Some of these methods
            were published before 1980 and required extraction with diethyl ether before
                                    1
            derivatisation and GC analysis.  Therefore new methods need to be developed that
            can be applied to foodstuffs especially desserts.


            14.4  References
             1 ‘Gas-liquid chromatographic determination of adipic acid in crackling candy and soft
               drinks’, Ito Y, Ogawa S, Iwaida M. J. Assoc. Off. Anal. Chem. (1979) 62(4), 937–938.
             2 ‘Determination of organic acids in foods by ion-exclusion chromatography’, Fujimura
               K, Tsuchiya M. Bunseki Kagaku (1998) 37(10), 549–553. [Japanese]
             3 ‘Measurements of urinary adipic acid and suberic acid using high-performance liquid
               chromatography’, Yoshioka K, Shimojo N, Nakanishi T, Naka K, Okuda K. Journal of
               Chromatography B (1994), 655, 189–193.
             4 ‘Determination of organic acids in food samples by capillary zone electrophoresis’,
               Klampfl C W, Buchberger W, Haddad P R. Journal of Chromatography A (2000) 881(1–
               2), 357–364.
             5 ‘Specific migration testing with alternative fatty food simulants’, Cooper I, Goodson A,
               OBrien A. Food Additives and Contaminants (1998) 15, 72–78.
             6 ‘Determination of adipic acid esters potentially migrated from plastic films for food-
               wrapping by gas chromatography and gas chromatography combined with mass
               spectrometry’, Katase T, Kim Y. Bunseki Kagaku (1999) 48(6), 649–655. [Japanese]
             7 ‘Phthalate and adipate esters in Australian packaging materials’, Balafas D, Shaw K J,
               Whitfield F B. Food Chemistry (1999) 65, 279–287.
             8 ‘Statistical evaluation of an international collaborative study concerning the improved
               gas chromatographic determination of adipate in starch’, Brunt K, Mitchell G A. Starch/
               Stärke (1997) 49, 296–301.
             9 ‘Improved method for the determination of total adipyl content in acetylated adipyl
               cross-linked starches’, Sanders P, Brunt, K. Starch/Stärke (1994) 46, 255–259.
            10 ‘Gas chromatographic determination of free adipic acid in adipyl cross-linked starches’,
               Sanders P, Brunt, K. Starch/Stärke (1996) 48, 448–452.
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