A gas chromatographic (GC) method has been developed for determination of cholesterol in meats. The method involves (a) ethanolic KOH saponification of the sample material, (b) homogeneous-phase toluene extraction of the unsaponifiables, (c) derivatization of cholesterol to its trimethylsilylether, and (d) quantitation by GC-flame ionization detection using 5-α-cholestane as internal standard. This direct saponification method is compared with the current AOAC official method for determination of cholesterol in 20 different meat products. The direct saponification method eliminates the need for initial lipid extraction, thus offering a 30% savings in labor, and requires fewer solvents than the AOAC method. It produced comparable or slightly higher cholesterol results than the AOAC method in all meat samples examined. Precision, determined by assaying a turkey meat sample 16 times over 4 days, was excellent (CV = 1.74%). Average recovery of cholesterol added to meat samples was 99.8%.
An international collaborative study was conducted on an HPLC method with fluorescent detection (FLD) for the determination of flavanols and procyanidins in materials containing chocolate and cocoa. The sum of the oligomeric fractions with degree of polymerization 1-10 was the determined content value. Sample materials included dark and milk chocolates, cocoa powder, cocoa liquors, and cocoa extracts. The content ranged from approximately 2 to 500 mg/g (defatted basis). Thirteen laboratories representing commercial, industrial, and academic institutions in six countries participated in the study. Fourteen samples were sent as blind duplicates to the collaborators. Results from 12 laboratories yielded repeatability relative standard deviation (RSDr) values that were below 10% for all materials analyzed, ranging from 4.17 to 9.61%. The reproducibility relative standard deviation (RSD(R)) values ranged from 5.03 to 12.9% for samples containing 8.07 to 484.7 mg/g. In one sample containing a low content of flavanols and procyanidins (approximately 2 mg/g), the RSD(R) was 17.68%. Based on these results, the method is recommended for Official First Action for the determination of flavanols and procyanidins in chocolate, cocoa liquors, powder(s), and cocoa extracts.
The aluminum content of 26 different foods was determined before and after the foods were cooked in uncoated new, conditioned and old aluminum pans, in stainless steel pans or in disposable aluminum trays and foil. All the foods tested contained small amounts of aluminum naturally. Some foods (i.e., potatoes boiled in new aluminum pans; cabbage and beef roasts cooked in aluminum pressure cookers; applesauce and eggs cooked in conditioned aluminum pans; tomatoes cooked in old aluminum pans; and mashed potatoes frozen and heated in TV dinner trays) accumulated significant (P<0.05) amounts of aluminum during preparation. However, the actual amounts of aluminum that were added to foods through the use of aluminum utensils were quite small as compared to the average dietary intake of aluminum by Americans.
Vitamin D is a fat-soluble vitamin with great nutritional interest. An HPLC/MS/MS method was developed to measure vitamin D with atmospheric pressure chemical ionization. Under the experimental parameters used, the LOQ was 0.018 IU/g or 0.45 ng/g, which greatly enhances the capability of measurement of vitamin D at low levels in foods and supplements. This method was validated with spike recovery of 100 15 and the RSD of less than 10 for most sample matrixes, including infant formula, cheese, cereal and cerealbased foods, multivitamin supplements, and pet foods. The results for vitamin D were compared with those obtained by other methods.
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