One hundred eighty-three suspect bear bile used in medicinal products, collected in Taiwan as gall bladders or dried powder forms, were analyzed using FTIR, HPTLC, and HPLC techniques to identify whether they are indeed bear bile. Those confirmed were further examined to determine whether the observed analytical parameters can be reliably used for source inference, i.e., differentiating products among North American black bear, farmed Asiatic black bear, polar bear, etc. Our data suggested that North American and polar bears contain a higher concentration of TC (relative to TUDC and TCDC), whereas the relative concentration of TC in Asiatic bears (wild or farmed) is much lower. Thus, the relative concentration of TC can potentially be used for differentiating Asiatic bear bile from North American and polar bear products, but it cannot be used for the differentiation of wild and farmed bear bile as suggested in an earlier report by Espinoza et al. The origin of the 183 samples analyzed were found to be as follows: 118 (64%), bile salts, or gall bladders were of domestic pig; 56 (31%), bile products of Asiatic bear; 4 (2.2%), Asiatic bear mixed with pig bile salts; 3 (1.6%) goat gall bladders; 1 (0.55%) water buffalo bile salts; and 1 (0.55%), pig bile salts mixed with water buffalo bile salts.
Two hundred and twenty-three vitreous humor specimens, which were obtained from a medical examiner's office, were found to be opiate positive (cutoff, 50 ng/mL) by fluorescence polarization immunoassay. All samples were analyzed for their free codeine, morphine, and 6-acetylmorphine contents by a gas chromatography-mass spectrometry protocol. 6-Acetylmorphine was found (cutoff, 10 ng/mL) in 41 specimens in the concentration range of 10-125 ng/mL. Twenty specimens had a free codeine-free morphine concentration ratio > or = 1. Eighty-five samples that were found to contain 50 ng/mL free morphine were further analyzed for their total codeine and total morphine contents. Total codeine-total morphine concentration ratios in 8 (of the 85 samples) were > or = 1, whereas this ratio in the others (only those with a codeine concentration high than 15 ng/mL were included) was significantly lower than 1. The codeine-morphine concentration ratio in vitreous humor appears to resemble that reported for blood and urine and can be used as the basis for differentiating between codeine- and morphine- (heroin-) induced fatalities.
Urine samples collected from one laboratory volunteer and five alleged heroin addicts are prepared (without preservatives) in 5-mL aliquots in glass culture tubes and stored at room, refrigerator, and freezer temperatures. Total morphine, total codeine, free morphine, and free codeine in these samples are analyzed at 30-day intervals for an 11-month period. Total morphine and total codeine concentration decreases are observed for all specimens in all storage conditions. For samples stored in the refrigerator and freezer, similar concentration decrease patterns are observed for total morphine and total codeine, and the decreases range from approximately 10 to 40%. The concentrations of free morphine and free codeine show slight but steady increases. For samples stored at room temperature, large decreases of total morphine are observed for three out of 10 specimens, and total codeine and total morphine concentrations (in seven other specimens) show a decrease pattern similar to that observed for the freezer and refrigerator storage conditions. Three concentration change patterns are observed for free morphine: The type I pattern follows the same decrease pattern observed for freezer and refrigerator storage conditions; the type II pattern shows free morphine increases (after 30-90 days of storage) that remain relatively high for the entire 11-month period; and the type III pattern shows initial increases, followed by gradual decreases to levels that are comparable with the specimens' respective initial concentrations. Free codeine concentrations show slight and steady increases for the entire 11-month period in all specimens.
A rapid, sensitive, and accurate stability-indicating high-performance liquid chromatographic assay method for determining the degradation of carprofen (CPF) is developed and validated under acidic, basic, or photo-irradiated conditions. The analysis is monitored with a Cosmosil 5C18-AR column using a mobile phase of CH3CN-H2O-AcOH (50:49:1, v/v/v) at 260 nm. The developed method satisfies the system suitability criteria, peak integrity, and resolution among the parent drug and its degradation products. The results indicate that the established assay method shows good selectivity and specificity suitable for stability measurements of CPF. CPF is found to be more sensitive to exposure to light and in acidic conditions, but it is stable in a basic medium. The kinetic study of the photodegradation of CPF follows an apparent first-order reaction in a variety of solvents. The solvent effects on the rates of degradation are in the decreasing order of chloroform > dichloromethane > methanol > ethanol > 2-propanol, which is irrelevant to the dielectric constant epsilon. However, the hydrogen-donating ability of the solvents is essential to the photochemical decomposition of CPF. A plot of log k versus the Kirkwood function exhibits a linear relationship in aqueous ethanolic solutions, which implies that degradation proceeds via an ionic mechanism.
The selective adsorption of d- or l-mandelic acid on starch from an aqueous solution of racemate has been quantitatively investigated. l-Mandelic acid has been judged from the distinct negative value of the optical rotation in the solution to be adsorbed preferentially over the d-isomer. The separation factor for the adsorption of the two enantiomers was 1.06±0.02 at 0°C. From the saturation value estimated by the Langmuir equation for adsorption, the ratio of the glucose residue to the Dl-mandelic acid adsorbed has been calculated as 5, indicating that not all the glucose residues in the starch constitute adsorption sites for mandelic acid.
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