Melamine has been used for the adulteration of cereal flours in order to increase their apparent protein content. Crude melamine may contain several by-products, i.e. ammeline, ammelide, and cyanuric acid. The simultaneous analysis of all four chemicals is difficult because of the formation of an insoluble salt between melamine and cyanuric acid. A simple and convenient high-performance liquid chromatography (HPLC) method for the detection of the adulteration of cereal flours with all four chemicals is proposed herein. The precipitate formation between melamine and cyanuric acid was prevented by using alkaline conditions (pH 11-12) for both standards preparation and sample extraction. The method uses matrix-matching, which involves the construction of a calibration curve on a blank (negative control) matrix, which is then used for the quantitation of melamine and by-products in adulterated (positive) samples. Matrix-matching compensates for analyte losses during sample preparation, and for matrix effects. The method was successfully applied to wheat, corn, and rice flours, and is expected to be applicable (with some modifications) to soy flour as well. The method allows for the detection of melamine, ammeline, and ammelide at approximately 5 microg g(-1), and cyanuric acid at approximately 90 microg g(-1) in wheat flour.
Spoilage of fruit juice by Alicyclobacillus acidoterrestris is characterized by a distinct medicinal or antiseptic off odor attributed to guaiacol, a metabolic by product of the bacterium. Detection of low populations of A. acidoterrestris that would precede sensory detection of guaiacol would enable juice processors to select appropriate processing and storage conditions that would minimize or eliminate spoilage. The objective of this study was to determine the recognition threshold of guaiacol in apple juice by sensory analysis and the population of A. acidoterrestris and incubation time at 21 and 37 degrees C necessary for chemical detection of guaiacol. Commercially sterilized apple juice (pH 3.54 +/- 0.04, 11.3 +/- 0.3 degrees Brix) was inoculated with a five-strain mixture of A. acidoterrestris spores (2.98 log10 CFU/ml) and stored at 21 or 37 degrees C for up to 61 days. Using an experienced sensory panel and the forced-choice ascending concentration method of limits, the best estimate threshold (BET) for recognition of guaiacol added to uninoculated apple juice was 2.23 ppb. Numbers of A. acidoterrestris spores and cells in inoculated juice remained constant during the 61-day storage period; however, the panel detected (P < or = 0.01) guaiacol in juice stored at 37 degrees C within 8 days. At three of four sampling times ranging from 13 to 61 days at which the sensory panel detected (P < or = 0.001) guaiacol, concentrations of 8.1 to 11.4 ppb were detected by chromatographic analysis. The panel detected (P < or = 0.1 to P < or = 0.01) guaiacol in five samples stored at 21 to 37 degrees C for 8 to 61 days in which the compound was not detected by chromatographic analyses. It appears that guaiacol content in apple juice inoculated with A. acidoterrestris is not always correlated with numbers of cells, and the limit of sensitivity of chromatographic quantitation of the compound is higher than the BET.
U.S. nutrition labeling regulations require the declaration of sodium content on food products. Accurate and reproducible determination of Na in foods with low Na content (<140 mg/serving) is challenging because of laboratory contamination. Within-laboratory performance of inductively coupled plasma/MS (ICP/MS), flame atomic absorption spectrophotometry (FAAS), ion-selective electrode (ISE), and potentiometric titration of chloride ion were evaluated in 17 low-sodium foods. For 13 types of food, statistically significant differences (P < 0.05) exist between the within-day and/or interday means obtained by ICP/MS, FAAS, and ISE. Median within-day and interday precent RSD values were 2.7 and 6.1, 3.5 and 3.2, and 5.6 and 6.2, respectively, by ICP/MS, FAAS, and ISE. The fewest matrix effects were found with ICP/MS, followed by FAAS, and ISE. FAAS gave higher results in a variety of matrixes when compared to ICP/MS and/or ISE. ISE did not perform well in fatty foods or at very low Na concentrations. Manufacturers' Nutrition Facts Panel sodium declarations exceeded levels found by analysis in >70 of the foods. Analysis of chloride content does not produce reliable Na estimates in low-sodium foods, even when added sodium chloride is present. Methodological issues and contamination sources are discussed.
An alternative, rapid, and reproducible method of analysis for perchlorate in selected food products (fruit and vegetable juice, milk, and bottled water) was developed and validated. Improvements over previous methods were achieved by the use of a rugged and inexpensive C18 column, a multi-mode OASIS HLB solid-phase extraction cartridge for sample clean-up, and acetic acid for pH adjustment and protein precipitation. The hydrophobicity of the perchlorate anion gives it good retention and separation characteristics on C18 chromatographic columns. The C18 column allowed for the use of 90% of acetonitrile at a low flow rate (0.3 ml min(-1)), without splitting, and could also be regenerated with organic solvents, unlike an ion-exchange column. Perchlorate levels in selected commercial food samples were: <1.0-2.1 ng g(-1) (fruit and vegetable juices, reported here for the first time), <1.0-5.0 ng g(-1) (milk), and <1.0 ng g(-1) (bottled water).
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