A closed vessel microwave digestion procedure was developed for shellfish samples. This procedure was compared with wet and dry ash procedures for levels of lead, cadmium, chromium, copper, and zinc. Results obtained for microwave and conventional wet ash digestion were comparable. The dry ashing procedure produced results consistently lower than either of the other methods. Recoveries ranged from 80-92% for microwave and wet ashing procedures and 54-72% for the dry ashing procedure. Accuracy was also determined by analyzing lobster hepatopancreas marine reference material. Values for Pb, Cd, and Cr fell within the range specified for the reference material for all 3 digestion procedures; however, values were lower for Cu and Zn. Results of this study show that microwave digestion is comparable to wet ashing. 相似文献
Radioactivity in soils labelled with 14C was determined by suspending the finely ground soil in a thixotropic gel, dispersing it by ultrasonics and counting the dispersion in a liquid scintillation spectrometer. The relationship between the weight of sample and counting efficiency was found to be almost linear. Using 30 mg soil, the counting efficiency is 50 per cent and 14C may be determined with an average coefficient of variation of 1.5 per cent to within 5 per cent of the value determined by oxidative procedures. 相似文献
Fluxes of 28 elements to Lake Michigan are calculated from literature data on sedimentation rates and concentrations in sediments and water. Lake Michigan residence times are roughly 104 lower than oceanic residence times. A mass balance has been formulated for 24 elements, with soil and aerosol as the only sources. These sources provide fourfold excesses of Cu, Hg, Sb, Se, and V, and order of magnitude deficits for Ca, Mg, Na, and Cl, but account (to within 50%) for the observed inputs of Ag, Al, As, Br, Co, Cr, Fe, K, La, Mn, S, Si, Sc, Th, and Zn. Except for Al, Co, La, Si, and Th, deposition from aerosol accounts for at least one-fifth of the total input. 相似文献
A method is described to determine acid and alkaline phosphatase activities from the rate of decomposition of p-nitrophenylphosphate in the presence of large amounts of organic matter, such as occur in the surface layers of soils or in animal wastes. The p-nitrophenol formed is separated by high pressure liquid chromatography on a cellulose column from p-nitrophenylphosphate and other organic compounds present in the soil or waste extract. After separation, p-nitrophenol is measured on-line in a spectrophotometric flow cell at a wavelength of 405 nm. In this way p-nitrophenol concentrations down to 0.1 μm can be measured, making it possible to work with substrate concentrations of 1 μm.
The necessity of correcting the phosphatase activity measured in this way for adsorption of enzyme, substrate (p-nitrophenylphosphate) and product (p-nitrophenol) is discussed.
Acid and alkaline phosphatases are inhibited strongly at phosphate concentrations greater than 0.1 mm, consequently substrate concentrations in the range of 0.01 to 0.1 mm were used.
The method was applied to a number of sandy soils and to pig slurry. Air drying or freeze drying of soils was found to decrease the phosphatase activity. Freeze drying did not affect the phosphatase activity of pig slurry. Michaelis-Menten kinetics were found to apply reasonably well. The resulting kinetic parameters are compared with values from the literature. Phosphatase activities are correlated with organic P and organic matter contents of soils and pig slurry. 相似文献
The determination of protein nitrogen in feeds and wheat by microcomputer controlled titration is described. The method involves direct titration of ammonia with standard hypochlorite titrant in the presence of bromide. The titrant is delivered by an automatic buret, and the microcomputer controlled, automatically computed potentiometric end points are precise to 0.1% over a 5-fold concentration range of nitrogen. Digestions performed with both mercury and copper catalysts show comparable results. Samples are weighed before digestion by an electronic balance interfaced to the computer which records sample number and weight. An automatic pipet aliquots, dilutes, and buffers samples directly from the digestion tubes; the samples can be immediately titrated with the automatic titrator. The results for protein in NBS standards and check feed samples from an offical testing program compare closely with average values reported for these standards. Results show that feed and wheat samples contained 10-100% protein. Precision for successive aliquots of the same digests is 0.1-0.4%relative standard deviation; precision for multiple digestions of the same sample is 0.1-0.8%. 相似文献
The characterization of herbal materials is a significant challenge to analytical chemists. Goldenseal (Hydrastis canadensis L.), which has been chosen for toxicity evaluation by NIEHS, is among the top 15 herbal supplements currently on the market and contains a complex mixture of indigenous components ranging from carbohydrates and amino acids to isoquinoline alkaloids. One key component of herbal supplement production is botanical authentication, which is also recommended prior to initiation of efficacy or toxicological studies. To evaluate material available to consumers, goldenseal root powder was obtained from three commercial suppliers and a strategy was developed for characterization and comparison that included Soxhlet extraction, HPLC, GC-MS, and LC-MS analyses. HPLC was used to determine the weight percentages of the goldenseal alkaloids berberine, hydrastine, and canadine in the various extract residues. Palmatine, an isoquinoline alkaloid native to Coptis spp. and other common goldenseal adulterants, was also quantitated using HPLC. GC-MS was used to identify non-alkaloid constituents in goldenseal root powder, whereas LC-MS was used to identify alkaloid components. After review of the characterization data, it was determined that alkaloid content was the best biomarker for goldenseal. A 20-min ambient extraction method for the determination of alkaloid content was also developed and used to analyze the commercial material. All three lots of purchased material contained goldenseal alkaloids hydrastinine, berberastine, tetrahydroberberastine, canadaline, berberine, hydrastine, and canadine. Material from a single supplier also contained palmatine, coptisine, and jatrorrhizine, thus indicating that the material was not pure goldenseal. Comparative data for three commercial sources of goldenseal root powder are presented. 相似文献
Population size is a major determinant of extinction risk. However, controversy remains as to how large populations need to be to ensure persistence. It is generally believed that minimum viable population sizes (MVPs) would be highly specific, depending on the environmental and life history characteristics of the species. We used population viability analysis to estimate MVPs for 102 species. We define a minimum viable population size as one with a 99% probability of persistence for 40 generations. The models are comprehensive and include age-structure, catastrophes, demographic stochasticity, environmental stochasticity, and inbreeding depression. The mean and median estimates of MVP were 7316 and 5816 adults, respectively. This is slightly larger than, but in general agreement with, previous estimates of MVP. MVPs did not differ significantly among major taxa, or with latitude or trophic level, but were negatively correlated with population growth rate and positively correlated with the length of the study used to parameterize the model. A doubling of study duration increased the estimated MVP by approximately 67%. The increase in extinction risk is associated with greater temporal variation in population size for models built from longer data sets. Short-term studies consistently underestimate the true variances for demographic parameters in populations. Thus, the lack of long-term studies for endangered species leads to widespread underestimation of extinction risk. The results of our simulations suggest that conservation programs, for wild populations, need to be designed to conserve habitat capable of supporting approximately 7000 adult vertebrates in order to ensure long-term persistence. 相似文献
Extraction of pigments (chlorophylls and carotenoids) from marjoram (Origanum majorana L.) with supercritical carbon dioxide was investigated. The aim of this study was to map the effects of extraction pressure and temperature on the yield of coloring materials by applying a 3(2) full factorial design with three repeated tests in the center of the design. For comparison, laboratory and pilot plant Soxhlet extractions were carried out using ethanol and n-hexane solvents. The compositions of pigments in marjoram extracts were determined by HPLC. Similar amounts of carotenoids, in addition to 40% of chlorophylls and their derivatives, were recovered from the supercritical fluid extraction, in comparison to the ethanol Soxhlet extraction. 相似文献
The oyster mushroom (Pleurotus ostreatus) is widely cultivated on wheat straw (Triticum aestivum); however, there is a need to better understand the relationship between the chemical composition of the compost and mushroom growth. Wheat straw was degraded over a period of 63 days by P. ostreatus during which time it was sampled at weekly intervals. Off-line thermochemolysis with tetramethylammonium hydroxide and solid-state (13)C NMR were then used in the molecular characterization of the undegraded wheat straw and the degraded samples. The degraded wheat straw samples had a lower proportion of syringyl- to guaiacyl-derived moieties and cinnamyl- to guaiacyl-derived moieties than the undegraded control. There were increases in both guaiacyl and syringyl acid to aldehyde ratios with composting time, which showed that side-chain oxidation has been mediated by P. ostreatus. The (13)C NMR spectra confirmed the increase in carboxyl content but indicated that the overall lignin and methoxyl contents remained relatively constant, although some nonsystematic variations were observed. The spectra also showed a decrease in amorphous noncellulosic polysaccharides in relation to the crystalline cellulose upon degradation. 相似文献