Page 303 - Analytical method for food addtives

202 Analytical methods for food additives

19.4 References
1 ‘Sucrose acetate isobutyrate (SAIB): Historical aspects of its use in beverages and a
review of toxicity studies prior to 1988’, Reynolds R C, Chappel C I. Food and Chemical
Toxicology (1998), 36(2), 81–93.
2 ‘Gas–liquid chromatographic estimation of sucrose diacetate hexaisobutyrate in soft
drinks’, Conacher H B S, Chadha R K. Journal of the AOAC (1972) 55(3), 511–513.
3 ‘Determination of sucrose diacetate hexaisobutyrate in soft drinks by gas–liquid
chromatographic analysis of isobutyric and acetic acid components as decyl esters’,
Conacher H B S, Chadha R K, Iyengar J R. Journal of the AOAC (1973) 56(5), 1264–
1266.
4 ‘Determination of sucrose esters of fatty acids in food additive premixes by gas
chromatography and confirmation of identity by gas chromatography/mass
spectrometry’, Uematsu Y, Hirata K, Suzuki K, Iida K, Kan T, Saito K. Journal of AOAC
International (2001) 84(2), 498–506.

19.5 Appendix: method procedure summary

Analysis of food additive premixes 4

Sample preparation

Method 1 – An SPE RP-select B column was washed with 10 mL methanol and
10 mL water successively before sample solution was transferred to the column. A
1.0 g portion of sample was dissolved in 5–10 mL of water–methanol (1:1). A
1 mL aliquot of the sample solution (<2 mg total SAIB) was transferred to the
column and the column was washed with 10 mL water–methanol (1:1). SAIB was
eluted with 10 mL methanol–THF (1:1). The fraction was evaporated to dryness
under reduced pressure and acetylated with 0.5 mL pyridine and 0.5 mL acetic
anhydride for 30 min at 35 ºC. After evaporation of the reagents under a nitrogen
stream, the residue was dissolved in 2 mL ethyl acetate. A 1 µL aliquot of the ethyl
acetate solution was injected into the gas chromatograph.
Method 2 – The solid sample was ground to a powder. A 1.0 g portion of sample
(powder, liquid or cream) was extracted twice with 50 mL THF. The THF phases
were filtered and concentrated to 20 mL under reduced pressure to prepare a
sample solution for column chromatography. A silica gel column was washed with
10 mL diethyl ether–ethyl acetate (3:7) before the sample solution was transferred
to the column. An aliquot of the sample solution (<2 mg SAIB) was evaporated to
dryness with a stream of nitrogen. The residue was transferred to the column with
a small amount of diethyl ether–ethyl acetate (3:7). SAIB was eluted with 10 mL
diethyl ether–ethyl acetate (3:7). The SAIB fraction was evaporated to dryness
under reduced pressure, and the residue was dissolved in 2 mL ethyl acetate. A
1 µL aliquot of the ethyl acetate solution was injected into the gas chromatograph.
Method 1 was applied to samples that were soluble in water–methanol (1:1) and
contained diglycerides (DG). Method 2 was applied to samples that were not
soluble in water–methanol (1:1) or to samples that contained DG.