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221.
Summary In this study, a rapid and efficient semi-micro extraction procedure is presented for the extraction of some higher n-alkanes
from water and soil samples. In the case of water samples n-hexane was used as the organic phase in a phase volume ratio (volume
of aqueous phase/volume of organic phase) higher than 285, while in the case of soil samples, extraction with n-hexane was
carried out in the presence of an excess of 2 M NaCl solution. The extraction rate from soil samples is very high and is better
than Soxhlet extraction, comparable with supercritical fluid extraction. High preconcentration factor in water samples allows
the limits of detection to be in the ng.mL−1 level with the use of gas chromatographic analysis. Flame ionization detector was used for monitoring the analytes. The obtained
recoveries of all studied compounds from both water and soil samples are higher than 90%. This method was successfully used
to determine some n-alkanes in municipal wastewater and contaminated soil. 相似文献
222.
The performance of ultrasonic and Soxhlet extraction using hexane, dichloromethane, ethylacetate/methyl-tert-butylether (1/3, v/v) and hexane/acetone (1/1, v/v) for the analysis of seventeen insecticides in sediments was evaluated. The contents of the extracts differed severely. The extracts obtained with ethylacetate/methyl-tert-butylether (1/3, v/v) and hexane/acetone (1/1, v/v) were dark yellow to green, whereas the extracts obtained with dichloromethane and hexane were light yellow and clear respectively. This is due to higher solubility of matrix compounds in ethylacetate/methyl-tert-butylether (1/3, v/v) and hexane/acetone (1/1, v/v). High loads of coextracted matrix compounds lead to matrix effects in the evaporation step of GC–MS measurements. This is known as matrix induced response enhancement effect. Matrix effects and recoveries were checked by analysis of spiked sediments. The suitable choice of extraction method in connection with an appropriate solvent separates the analytes from matrix compounds. Matrix effects are reduced and recoveries of spiked samples are improved.Revised: 6 January and 2 May 2005 相似文献
223.
Jun Ping Xiao Qing Xiang Zhou Hua Hua Bai Department of Chemistry University of Science Technology Beijing Beijing China School of Chemistry Environmental Sciences Henan Normal University Henan Key Laboratory for Environmental pollution Control Xinxiang China 《中国化学快报》2007,18(6):714-717
A procedure for the preconcentration of copper was described in this paper using multi-walled carbon nanotubes (MWCNTs) oxidized by potassium permanganate as the adsorbent for the enrichment of trace copper in water samples. Important parameters, such as the sample pH, the concentration and volume of eluent, sample flow rate and volume, and interference of coexisting ions, were investigated. The obtained results indicated that proposed method possessed an excellent analytical performance. The linear range, the detection limit, and precison (RSD) were 1-100 ng/mL (R2 = 0.9993), 0.32 ng/mL and 2.88%, respectively. The results showed that copper could be adsorbed quantitatively on the pretreated MWCNTs with potassium permanganate, and proposed method was very useful in the monitoring of copper in the environment. 相似文献
224.
A fully automated flow-through microcolumn fractionation system with on-line post-extraction derivatization is proposed for monitoring of orthophosphate in solid samples of environmental relevance. The system integrates dynamic sequential extraction using 1.0 mol l−1 NH4Cl, 0.1 mol l−1 NaOH and 0.5 mol l−1 HCl as extractants according to the Hieltjes-Lijklema (HL) scheme for fractionation of phosphorus associated with different geological phases, and on-line processing of the extracts via the Molybdenum Blue (MB) reaction by exploiting multisyringe flow injection as the interface between the solid containing microcolumn and the flow-through detector. The proposed flow assembly, capitalizing on the features of the multicommutation concept, implies several advantages as compared to fractionation analysis in the batch mode in terms of saving of extractants and MB reagents, shortening of the operational times from days to hours, highly temporal resolution of the leaching process and the capability for immediate decision for stopping or proceeding with the ongoing extraction. Very importantly, accurate determination of the various orthophosphate pools is ensured by minimization of the hydrolysis of extracted organic phosphorus and condensed inorganic phosphates within the time frame of the assay. The potential of the novel system for accommodation of the harmonized protocol from the Standards, Measurement and Testing (SMT) Program of the Commission of the European Communities for inorganic phosphorus fractionation was also addressed. Under the optimized conditions, the lowest detectable concentration at the 3σ level was ≤0.02 mg P l−1 for both the HL and SMT schemes regardless of the extracting media. The repeatability of the MB assay was better than 2.5% and the dynamic linear range extended up to 7.0 mg P l−1 in NH4Cl and NaOH media and 15 mg P l−1 whenever HCl is utilized as extractant for both the HL and SMT protocols. 相似文献
225.
Raman spectra of intramolecular vibration mode for each guest species in the methane + tetrafluoromethane (CF4) mixed-gas hydrate crystal have been measured at 291.1 K. Both of pure guest species generate the structure-I hydrate in the present pressure ranges. Isothermal phase-equilibrium curve exhibits two discontinuous points around the equilibrium methane compositions (water-free) in the gas phase of 0.3 and 0.8. At the above points, the Raman spectra of both guest molecules have been drastically changed. One of the most important findings is that the crystal of methane + tetrafluoromethane mixed-gas hydrate shows the structural phase-transition (from the structure-I to the structure-II and back to the structure-I) caused by composition changes. 相似文献
226.
Rozhon W Petutschnig E Wrzaczek M Jonak C 《Analytical and bioanalytical chemistry》2005,382(7):1620-1627
Salicylic acid (SA) is an important signaling compound in plants and is involved in various defense responses. Here we report a new method for quantification of free and total soluble SA in Arabidopsis thaliana with 5-fluorosalicylic acid (5-FSA) as internal standard. The SA was isolated from leaf extracts by solid-phase extraction with phenyl-phase cartridges and selectively eluted as the cationic iron(III)-complex. Recoveries of SA and 5-FSA were equal and exceeded 90%. Free SA was subsequently released from the iron(III)-complex by addition of 2,2-bipyridyl and high-performance anion-exchange chromatography was performed on an NH2 column. The SA appeared as last peak with a retention time of 15 min, baseline-separated from other substances. On-line detection was performed fluorimetrically for both SA and 5-FSA at an excitation wavelength of 300 nm and an emission wavelength of 410 nm, because both substances give similar fluorescence spectra. The detection limit for SA was 5 ng g–1 FW for a sample size of 100 mg. Thus the main advantages of the method are highly selective sample preparation, increased sensitivity, reduced analysis time compared with reversed-phase HPLC, and use of a novel internal standard detectable under the same conditions as SA. The techniques described are applicable to other plant materials. 相似文献
227.
Quantitative analysis of docetaxel in human plasma using liquid chromatography coupled with tandem mass spectrometry 总被引:2,自引:0,他引:2
Kuppens IE van Maanen MJ Rosing H Schellens JH Beijnen JH 《Biomedical chromatography : BMC》2005,19(5):355-361
An assay for the quantitative determination of docetaxel in human plasma is described. Docetaxel was extracted from the matrix using liquid-liquid extraction with ter-butylmethylether, followed by high-performance liquid chromatographic analysis using an alkaline eluent. Paclitaxel was used as internal standard. Positive ionization electrospray tandem mass spectrometry was performed for selective and sensitive detection. The method was validated according to the FDA guidelines on bioanalytical method validation. The validated range for docetaxel was from 0.25--1000 ng/mL using 200 microL plasma aliquots. The method requires only a limited volume (200 microL) of human plasma and the method can be applied in studies requiring a low lower limit of quantitation of 0.25 ng/mL. The assay was applied successfully in several clinical and pharmacological studies with docetaxel. 相似文献
228.
超临界NaCl水溶液的分子动力学模拟 总被引:7,自引:0,他引:7
采用分子动力学模拟的方法对超临界NaCl水溶液的微观结构进行了研究.模拟发现在所研究超临界条件下,密度的变化比温度的变化对超临界NaCl水溶液的微观结构影响更大.温度及密度对Cl- H2O径向分布函数的影响比对Na+ H2O径向分布函数的影响要大.超临界条件下,各gNa+-Cl-在0.261 nm处出现峰值,表明Na+、Cl-之间发生了离子的缔合.超临界条件下,随温度增加,缔合作用增强;随密度增加,缔合作用减弱.本文工作为建立可适用于超临界条件下的电解质热力学模型提供了依据. 相似文献
229.
A solution-phase synthesis of bicyclic prolines containing four points of diversity has been developed by a two-step synthesis involving 1,3-dipolar cycloaddition of perfluoroalkylsulfonyl-protected hydroxybenzaldehydes followed by Pd-catalyzed Suzuki coupling reaction of fluorous sulfonates with boronic acids. Both reactions are conducted under microwave irradiation and reaction mixtures are purified by solid-phase extractions without performing chromatography. 相似文献
230.
Harro Lentz Ernst Ulrich Franck 《Angewandte Chemie (International ed. in English)》1978,17(10):728-730
Liquid or dense supercritical ammonia has been suggested as an extraction fluid. It is indeed good solvent for very different classes of compounds, as can be seen from phase diagrams. Such diagrams for binary systems of ammonia and hydrocarbons are presented and discussed on the basis of their critical curves. Apparatus and methods for the measurement of phase equilibria and equation of state data of fluid mixtures at high pressure are described. 相似文献