A collaborative study was conducted using a modified AOAC method (sugars in chocolate) for the determination of fructose, glucose, sucrose, and maltose in presweetened cereals by high pressure liquid chromatography (HPLC). Eight samples consisting of 6 products were analyzed in duplicate by the HPLC method and the AOAC Lane-Eynon method. The AOAC method was modified to use water-alcohol (1 + 1) and Sep-Pak C18 cartridges for sample cleanup. The HPLC results indicate precision comparable to the Lane-Eynon method and the chocolate method. The modified HPLC method has been adopted official first action.
The McCleary enzymatic assay for mixed linkage (1→3)(1→4)-beta-D-glucans has been modified to apply to oat and barley fractions and ready-to-eat (RTE) cereals. The proposed method involves lower sample concentrations; stirring the samples; a longer, warmer lichenase digestion; and longer beta-glucosidase digestion. These changes result in higher recovery of beta-glucan. This modification expands on the American Association of Cereal Chemists (AACC) Method 32-22 by the addition of a desugaring procedure, which is necessary for RTE cereals. Results from collaborative studies sponsored by AACC and AOAC demonstrate good precision for an enzymatic assay. The average relative standard deviation for reproducibility (RSDR, a measure of inter laboratory variation) for 20 oat, barley, and cereal samples was 9.7%. The average RSD for repeatability (RSDr, intralaboratory variation) was 5.0%. The enzymatic method has been adopted first action by AOAC International for determination of beta-glucans in oat and barley fractions, and ready-to-eat cereals.
A gas-liquid chromatographic method is described for the simultaneous determination of sorbic acid and sodium benzoate in table sirup. The preservatives are extracted from acidified sirup with ethyl acetate and are analyzed on a gas chromatograph equipped with a flame ionization detector and a glass column (4 ft × 4 mm id) containing 9% SP-1200 and 2% H3PO4 on Chromosorb W (AW). Coefficients of variation for sorbic acid and sodium benzoate are 0.62 and 0.41%, respectively. Analysis time is less than 20 min, with recoveries exceeding 90%.
A high performance liquid chromatographic (HPLC) method for vitamin D in pet foods and feeds at low concentrations (2-8 IU/g = 50-200 ppb) was studied collaboratively. The procedure consists of the following purification steps: saponification, extraction oMhe unsaponifiable fraction, chromatography on alumina, cleanup on reverse phase HPLC, and quantitation with straight phase HPLC. The original method, developed by Knapstein, was simplified by deleting the quantitative TLC step. Six coded samples were distributed to 31 laboratories, along with a known sample containing 15 IU/g to allow practice of the rather complicated procedure. Eighteen collaborators returned their results. Results for the spiked samples show good recovery. The estimates of repeatability and reproducibility are 0.96 and 2.2 IU/g for spiked samples and 1.5 and 3.1 IU/g for commercial samples, respectively, which are considered acceptable for these low concentrations. The method has been adopted official first action.
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