PubMed · 11008789
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T J Ward. 2000-09-15. Chiral separations.. https://doi.org/10.1021/ac000841o
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A fully computer-controlled apparatus was designed. It combines a glass reactor with a temperature-controlled hood, in which headspace volatiles are captured. Flavored liquids can be introduced into the reactor and exposed to conditions of temperature, air flow, shear rate, and saliva flow as they occur in the mouth. As the reactor is completely filled before measurements are started, creation of headspace just before sampling start prevents untimely flavor release resulting in real time data. In the first 30 s of flavor release the concentrations of the volatiles can be measured up to four times by on-line sampling of the dynamic headspace, followed by off-line trapping of the samples on corresponding Tenax traps and analysis using GC-TDS-FID. Flavor compounds from different chemical classes were dissolved in water to achieve concentrations typically present in food (micrograms to milligrams per liter). Most of the compounds showed constant release rates, and the summed quantities of each volatile of three 10 s time intervals correlated linearly with time. The entire method of measurement including sample preparation, release, sampling, trapping, thermodesorption, and GC analysis showed good sensitivity [nanograms (10 s)(-1)] and reproducibility (mean coefficient of variation = 7.2%).
Qualitative and quantitative analyses of N-heterocycle compounds were conducted by using a liquid-liquid extraction followed by additional chemical silica gel purification and injection into a gas chromatographic (GC) column coupled to a nitrogen-phosphorus detector (NPD). The purified extract fraction was investigated by GC-NPD and by GC-mass spectrometry. The compounds identified and quantified in wines were 2,4,5-trimethyloxazole, 2,4-dimethylthiazole, and 4-methylthiazole by GC-NPD and both 2-acetylthiazole and 2-acetyl-2-thiazoline by GC-MS. The procedure was used to analyze different wines and gave reliable and reproducible results.
A biological monitoring method for urinary dichloromethane (DCM) has been developed by using head-space gas chromatography with FID detection. The calibration curve is linear in a wide range of DCM levels between 0.01 and 2 mg/l. The recovery rate is almost 100% and within-run coefficients of variation are 2.9-3.7%. A highly significant correlation is found between exposure levels and urinary concentrations of DCM. Determination of urine DCM by this method has many advantages such as sample storage, no need for correction of urine concentration, absence of gender difference and also no confounding effect of glutathione S-transferase T1 polymorphism.