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51.
Analysis of Cembranoids in Flue‐cured Tobacco by Accelerated Solvent Extraction and Gas Chromatography‐Mass Spectrometry‐Selected Ion Monitoring 下载免费PDF全文
Xiao‐Bo Qian Jiang‐Ping Ye Xiao‐Ming Chen Chang‐Hua Zhang Yong‐Jiang Liang Zhang‐Hai Li Jun Yang 《中国化学会会志》2014,61(10):1133-1140
An efficient and sensitive analytical method based on accelerated solvent extraction (ASE) and gas chromatography‐mass spectrometry‐selected ion monitoring (GC‐MS‐SIM) was developed and validated for analysis of cembranoids in flue‐cured tobacco leaves. Extraction efficiency of different pretreatment methods including liquid‐solid extraction (LSE), ultrasound‐assisted extraction (UAE), Soxlet extraction and accelerated solvent extraction (ASE) was compared and ASE was chosen as the optimal extraction method. During ASE procedure, effect of four parameters on extraction efficiency was considered and the experimental conditions were selected as follows: extraction solvent: dichloromethane; oven temperature: 50 °C; static time: 5 min and number of cycles: 2. Working standards of cembranoids were isolated by silica gel column chromatography and the identification was performed by mass spectrometry. Performance characteristics such as linearity, limit of detection (LOD), limit of quantitation (LOQ), precision and recovery were studied. The LOD and LOQ values were ranging from 5.0 × 10?3 to 6.9 × 10?3 μg/mL and 1.7 × 10?2 to 2.3 × 10?2 μg/mL for all analytes. At three different spiked levels, recoveries for CBT‐ol, α‐CBT‐diol and β‐CBT‐diol were 94.6%‐105.1%, 93.0%‐97.2% and 88.7%‐107.5% while the relative standard deviations (RSDs) were in the ranges of 3.9%‐6.2%, 1.8%‐8.7% and 1.7%‐6.0%, respectively. The proposed analytical methodology was successfully applied in the analysis of cembranoids in tobacco samples. 相似文献
52.
Determination of pharmaceuticals in biosolids using accelerated solvent extraction and liquid chromatography/tandem mass spectrometry 总被引:1,自引:0,他引:1
An analytical method was developed to quantitatively determine pharmaceuticals in biosolid (treated sewage sludge) from wastewater treatment plants (WWTPs). The collected biosolid samples were initially freeze dried, and grounded to obtain relatively homogenized powders. Pharmaceuticals were extracted using accelerated solvent extraction (ASE) under the optimized conditions. The optimal operation parameters, including extraction solvent, temperature, pressure, extraction time and cycles, were identified to be acetonitrile/water mixture (v/v 7:3) as extraction solvent with 3 extraction cycles (15 min for each cycle) at 100 °C and 100 bars. The extracts were cleaned up using solid-phase extraction followed by determination by liquid chromatography coupled with tandem mass spectrometry. For the 15 target pharmaceuticals commonly found in the environment, the overall method recoveries ranged from 49% to 68% for tetracyclines, 64% to 95% for sulfonamides, and 77% to 88% for other pharmaceuticals (i.e. acetaminophen, caffeine, carbamazepine, erythromycin, lincomycin and tylosin). The developed method was successfully validated and applied to the biosolid samples collected from WWTPs located in six cities in Michigan. Among the 15 target pharmaceuticals, 14 pharmaceuticals were detected in the collected biosolid samples. The average concentrations ranged from 2.6 μg/kg for lincomycin to 743.6 μg/kg for oxytetracycline. These results indicated that pharmaceuticals could survive wastewater treatment processes, and accumulate in sewage sludge and biosolids. Subsequent land application of the contaminated biosolids could lead to the dissemination of pharmaceuticals in soil and water environment, which poses potential threats to at-risk populations in the receiving ecosystems. 相似文献
53.
M.L. Palma 《Molecular physics》2013,111(18):2163-2172
Following our previous study on spin–rotation and shielding constants of the SF6 molecule, the rotational g factor and the magnetic susceptibility are calculated here, using ab initio methods to evaluate the electronic contribution to the nuclear hyperfine constants, and compared with experimental results. It is shown, for the first time, that the electronic component of the rotational g factor is proportional to a constant, which is given by a sum over electronic states. We also evaluate for the SF6 molecule the indirect, or electron-coupled spin–spin interaction, theoretically described by Ramsey, and show that it gives non-negligible corrections to direct coupling constants d 1 and d 2. The contributions of the terms included in this interaction (DSO, PSO, SD and FC) are also analysed. 相似文献
54.
M. Celina A.B. Trujillo K.T. Gillen L.M. Minier 《Polymer Degradation and Stability》2006,91(10):2365-2374
Chemiluminescence (CL) has been applied as a condition monitoring technique to assess aging related changes in a hydroxyl-terminated-polybutadiene based polyurethane elastomer. Initial thermal aging of this polymer was conducted between 110 and 50 °C. Two CL methods were applied to examine the degradative changes that had occurred in these aged samples: isothermal “wear-out” experiments under oxygen yielding initial CL intensity and “wear-out” time data, and temperature ramp experiments under inert conditions as a measure of previously accumulated hydroperoxides or other reactive species. The sensitivities of these CL features to prior aging exposure of the polymer were evaluated on the basis of qualifying this method as a quick screening technique for quantification of degradation levels. Both the techniques yielded data representing the aging trends in this material via correlation with mechanical property changes. Initial CL rates from the isothermal experiments are the most sensitive and suitable approach for documenting material changes during the early part of thermal aging. 相似文献
55.
注入热焓法测定萃取磷酸中三氧化硫 总被引:1,自引:0,他引:1
以钡离子与硫酸根离子沉淀反应的热效应为基础,通过测定孤立体系中的温度变化,建立了测定萃取磷酸中三氧化硫的注入热焓法,该法在4.0-32.0g/L范围内可准确测定SO3的含量,相对标准偏差为1.8%;标准加入回收率为98%-103%。 相似文献
56.
Mieczysław Kozłowski Helena Wachowska Jan Yperman 《Central European Journal of Chemistry》2003,1(4):366-386
Products of reductive and non-reductive methylation of two high-sulphur coals (Mequinenza and Illinois No. 6) have been extracted
by dichloromethane. It has been established that the efficiency of the transformation of coal to the products soluble in CH2Cl2 is higher for coals subjected to non-reductive methylation by the Liotta method than for those after reduction in the potassium/liquid
ammonia system. The extracts and the extraction residues were subjected to elemental analysis, IR spectroscopy, and AP-TPR
(Atmospheric Pressure-Temperature Programmed Reduction) measurements. It has been shown that the main species undergoing extraction
by CH2Cl2 are aliphatic compounds or aromatic structures of low degree of condensation. The effect of the extraction on the sulphur
groups in coal has been discussed. 相似文献
57.
T. Kaljuvee A. Trikkel R. Kuusik V. Bender 《Journal of Thermal Analysis and Calorimetry》2005,80(3):591-597
Summary The results of investigation of MgO participation in the binding of SO2 with lime-containing materials as sorbents are presented. Experiments of SO2 binding into solid phase using model samples of reactive grade MgO and CaO varying the mole ratio of MgO/CaO from 9:1 to 1:9 were carried out. Besides, dolomite and limestone samples with different MgO/CaO mole ratio (from 1.24 to 0.13) and samples of ashes formed at combustion of Estonian oil shale (containing 35-40% of carbonates) and its semicoke were studied Initial samples, intermediate and final products were subjected to chemical, IR-spectroscopy, X-ray and BET specific surface area analyses. The results of the present study confirmed the active participation of MgO in the binding of SO2 into the solid phase. In addition to CaSO4 the formation of Ca,Mg-double sulphate CaMg3(SO4)4 and -MgSO4 was observed. The presence of CaMg3(SO4)4 was fixed in a large temperature range 400-900°C and that of -MgSO4 in between 500-700°C. The optimum temperature range for formation and durability of CaMg3(SO4)4 was 700-800°C. 相似文献
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Salt efflorescences consisting of gypsum sampled mainly in the Schirmacher Oasis have been analyzed for the isotopic composition of the water of crystallization and of the sulphate-sulphur. For comparison, a few samples from other Antarctic locations (Guettard Range, Prince Charles Mts., Insel Mts.) were included in the study. The isotopic variations of the water of crystallization of secondary gypsum and the calculated isotopic composition of the mother solution reflect the local climatic conditions during the precipitation of the efflorescences. It is therefore possible to obtain qualitative information about the climatic conditions prevailing in the studied region. 相似文献