Isoflavones are biologically active compounds occurring naturally in a variety of plants, with relatively high levels found in soybeans. Twelve laboratories participated in a collaborative study to determine the aglycon isoflavone content of 8 test samples of soy and foods containing soy. The analytical method for the determination of isoflavones incorporates a mild saponification step that reduces the number of analytes measured and permits quantitation versus commercially available, stable reference standards. Test samples were extracted at 65°C with methanol–water (80 + 20), saponified with dilute sodium hydroxide solution, and analyzed by reversed-phase liquid chromatography with UV detection at 260 nm. Isoflavone results were reported as μg/aglycon/g or μg aglycon equivalents/g. The 8 test samples included 2 blind duplicates and 4 single test samples with total isoflavone concentrations ranging from approximately 50 to 3000 μg/g. Test samples of soy ingredients and products made with soy were distributed to collaborators with appropriate reference standards. Collaborators were asked to analyze test samples in duplicate on 2 separate days. The data were analyzed for individual isoflavone components, subtotals of daidzin–daidzein, glycitin–glycitein, and genistin–genistein, and total isoflavones. The relative standard deviation (RSD) for repeatability was 1.8–7.1%, and the RSD for reproducibility was 3.2–16.1% for total isoflavone values of 47–3099 μg/g.
Lanthanum and yttrium trifluoromethanesulfonates at 1 mole % concentration, have been found to catalyze a reaction between ammonia and aromatic nitriles to yield symmetrically substituted 2,4,6‐triaryl‐s‐triazines. The generally high yields and relatively mild reaction conditions of this procedure suggest it as an alternative to other aromatic nitrile cyclotrimerization reactions. Of the aliphatic nitriles studied, acetonitrile and cyclopropanecarbonitrile gave good yields of triazine, propionitrile and butyronitrile gave significantly reduced yields of triazines 3b and 3c respectively. Rearrangement of 3a and 3b to alkylated‐4‐aminopyrimidines was observed.
Polyadipate plasticizers can be present in the polyvinylchloride (PVC) gaskets used to seal the lids of glass jars. As the gaskets can come into direct contact with the foodstuffs inside the jar, the potential exists for polyadipate migration into the food. The procedure and performance characteristics of a test method for the analysis of polyadipates in food simulants (3% aqueous acetic acid and 10% aqueous ethanol) and the volatile test media used in substitute fat tests (isooctane and 95% aqueous ethanol) are described. The PVC gaskets were exposed to the food simulants or their substitutes under standard test conditions. Studies were initially carried out using direct measurement of the polyadipate oligomers by liquid chromatography with time-of-flight mass spectrometric detection (LC-TOF-MS) but this was not practical due to the number of peaks detected. Instead, the migrating polyadipates were hydrolysed to adipic acid and measured by liquid chromatography with tandem mass spectrometric detection (LC-MS/MS). The amount of polyadipate that this measurement of adipic acid represents was then calculated. Method performance was assessed by analysis of gaskets from two types of jar lids by single-laboratory validation. Linearity, sensitivity, repeatability, intermediate reproducibility and recovery were determined to be suitable for checking compliance with the 30 mg/kg specific migration limits for polyesters of 1,2-propane diol and/or 1,3- and/or 1,4-butanediol and/or polypropylene-glycol with adipic acid, which may be end-capped with acetic acid or fatty acids C(12)-C(18) or n-octanol and/or n-decanol. The method was found to be much quicker than previous methods involving extraction, clean-up, hydrolysis, esterification, derivatisation and GC measurement, consequently saving time and money.
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