A method is proposed to assess deterioration of frying fats by measuring polar and nonpolar components separated on a silica gel column. Means for polar components measured in duplicate samples by 19 collaborators ranged from 8.0 ± 0.34 to 25.8 ± 0.90%. Coefficients of variation ranged from 3.5 to 4.9%. The method has been adopted as official first action.
The vitamin E group includes tocopherols and tocotrienols and their isomers, esters, and derivatives. They differ not only in biopotencies as antisterility agents but also in activities in other physiological and chemical relationships. Unlike vitamins A and D, foods (vegetable oils) are among the richest sources of vitamin E, and assay methods for vitamin E include food applications more often than for the former vitamins. Physicochemical methods are replacing bioassays for vitamin E and tocopherol wherever possible because of greater specificity and less variability, time, and, sometimes, expense. Unless careful purifications and isolations are carried out and some of the relative vitamin E activities of components are calculated, bioassays are still required for total vitamin E activity. The vitamin E group is separated by column, paper, thin-layer, gas-liquid, and high-pressure liquid chromatography (HPLC). Gas-liquid chromatography has been more successfully used for vitamin E than for other fat-soluble vitamins. Recently developed HPLC methods for vitamin E are sensitive and apparently require less cleanup of extracts and less time than former methods; HPLC may prove to be the most useful technique for vitamin E in foods, especially if other fat-soluble vitamins can be determined simultaneously on the same sample extract.
Criticisms have been voiced concerning the methods employed for determining the fatty acid composition of vegetable oils used in processing of fried foods. In the present study several different vegetable oils were heated under standardized conditions, at frying temperatures and under air, for various periods of time, and then subjected to analyses for fatty acid composition. The methods employed were : UV spectrophotometry; gas-liquid chromatography (GLC) employing either normalization of the peak areas, direct standards or internal standards ; and the enzymic, lipoxidase procedure. The present findings confirm that the drop in iodine value is a good approximation of the reduction of polyunsaturated fatty acids in heated oils. In evaluating liquid nonhydrogenated vegetable oils that had been subjected to heat abuse under standard conditions, all of the analytical methods for the estimation of fatty acid composition, with the exception of normalization of GLC peak areas, give substantially the same results. With hydrogenated vegetable oils, the analytical methods provide values which differ significantly among themselves. Evidence was also presented to show that the quantity of material retained on the gas chromatographic column is directly related to the loss of polyunsaturates for oils heated under controlled conditions. For evaluation of oils from frying operations, the preferred method is the GLC method utilizing internal standards if the purpose is the determination of total polyunsaturated fatty acids. However, if the study being made involves a question of nutritional value, then the measurement of the essential fatty acids by the lipoxidase enzymic procedure is the more valid method for evaluation of heated oils.
For more than a decade, numerous analytical methods have been proposed for the detection and measurement of polymers in vegetable fats and oils. Many of the methods have been little more than laboratory curiosities, either because they were concemed with only very specific compounds or were too cumbersome and time consuming to become very popular. More recently, a number of methods in common use for analysis of fats and oils has been shown to be useful for indirectly measuring polymeric materials in heat abused oils. The present report shows, by the use of gel filtration chromatography, the validity of two of the indirect methods of estimating polymeric products of abused fats and oils. These methods are: the estimation of polymers through changes in the iodine value and the measurement of retention materials on a gas liquid chromatographic column. A new simplified internal standard gas liquid chromatographic procedure utilizing triglyceride standards also is presented. This latter method permits estimating the degree of degradation of vegetable fats and oils by any laboratory capable of determining the fatty acid composition of a sample by gas liquid chromatography.
Aflatoxin analysis, with post-column derivatization using a photochemical reactor for enhanced detection (PHRED) system for derivatization, has been compared to the officially recognized iodine and Kobra cell derivatization systems. This photochemical system has been extensively used for screening peanuts by some U.S. Department of Agriculture laboratories for many years. From their periodic method checks, using standard spiked samples, an 80 sample series with each of the 3 derivatization methods was statistically analyzed. Paired comparisons, using the same sample extract, were also made between the PHRED and one of the other 2 methods, among laboratories in 4 different countries, on a variety of naturally contaminated commodity products. The differences between the techniques were not significant for peanuts, but for corn the photochemical system consistently gave slightly higher values for aflatoxins B1 and B2 than the Kobra cell method. However, a comparison of all sample results showed no significant differences between methods. The Pearson correlation coefficients for aflatoxin B1 in 102 test samples and aflatoxin B2 in 94 test samples were 0.9994 and 0.9874, respectively. The probability factor was P < 0.0001, and the t-tests were not significantly different except for the corn. These indicated that the PHRED system is equivalent to the iodine and Kobra cell methods for peanuts relative to the current official procedures, but the PHRED system has a slightly high bias for corn compared to the iodine and Kobra cell systems.
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