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D M Sullivan

Publications and source records attributed to D M Sullivan.

75 records · Page 5Linked to original sources

Measurement of trace levels of total aluminum in foods by atomic absorption spectrophotometry.

A graphite furnace atomic absorption spectrophotometry method was used to determine the total aluminum content of various foods found in an average American diet. The food products were ashed in platinum dishes, and the inorganic residue was fused using a sodium carbonate-sodium borate mixture. The fusion step allowed detection of all the various forms of aluminum found in food products. A L'vov platform was used in the graphite furnace to increase the sensitivity of the assay. Care was taken throughout the analysis to avoid various sources of aluminum contamination such as glass and porcelain dishes. All reagents were ultra-pure grade and were continuously monitored for aluminum content. Sodium borate used in the fusion flux mixture had previously been extracted with 8-hydroxyquinoline in chloroform to remove any aluminum present. Both raw and cooked foods were analyzed for aluminum with this method. Average recoveries of aluminum from food products ranged from 84 to 112%. The overall coefficient of variation of this method on the food products tested was 10%.

Aluminum↗

Determination of phytosterols in butter samples by using capillary column gas chromatography.

A positive bias in the gas chromatographic (GC) analysis of butter for beta-sitosterol was discovered when attempting to confirm values by gas chromatography/mass spectrometry (GC/MS). The source of the problem was traced to an interfering material that was not effectively separated by packed column GC. Because capillary columns are known to provide superior separation, they were substituted for packed columns in the assay, and instrument parameters were modified accordingly. A compound with a similar retention time, identified by GC/MS as lanosterol, was separated from beta-sitosterol by the capillary column. The capillary column technique was applied to over 300 butter samples. The results indicate that the method can accurately quantitate beta-sitosterol in butter with no known interferences. The limit of detection for this method is 1 mg/100 g. Recoveries at a level of 3 mg/100 g averaged 98% with a coefficient of variation of 3.45%.

Butter↗

Evaluation of direct saponification method for determination of cholesterol in meats.

A gas chromatographic (GC) method has been developed for determination of cholesterol in meats. The method involves ethanolic KOH saponification of the sample material, homogeneous-phase toluene extraction of the unsaponifiables, derivatization of cholesterol to its trimethylsilylether, and quantitation by GC-flame ionization detection using 5-alpha-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%.

Chemical Phenomena↗