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31.
WEI Wei LI Xu-wen SHI Xiao-lei ZHOU Hong-yu YANG Rui-jie ZHANG Han-qi JIN Yong-ri College of Chemistry Jilin University Changchun P. R. China 《高等学校化学研究》2011,27(1):23-27
Matrix solid-phase dispersion(MSPD) was developed for the extraction of four alkaloids, including aconitine, mesaconitine, hypaconitine and deoxyaconitine, from the roots of Aconitum kusnezoffii Reichb. The determination of the analyte was carried out by high performance liquid chromatography with UV detection. The alkaline alumina was used as sorbent. The mixture of acetonitrile and water was used as elution solvent. Several extraction parameters, such as type of sorbent, the ratio of sample to solid suppo... 相似文献
32.
Ioana Diaconu Hassan Y. Aboul-Enein Mohammed A. Al-Omar Gheorghe Nechifor Elena Ruse Andrei A. Bunaciu Eugenia Eftimie Totu 《Arabian Journal of Chemistry》2011,4(1):99-103
The paper presents experimental data obtained in the study of liquid–liquid partition equilibriums in biphasic system in order to optimize the process of transport through bulk liquid membranes (triphasic partition systems). The partition equilibriums of some nitrophenols using chloroform as extraction solvent and membranary solvent, respectively, were studied. The influence of the pH on the partition equilibriums was investigated. The repartition constants and the pKa values of the studied nitrophenols were calculated. Nitrophenols were transferred in triphasic system from a feed phase with pH 2, through a chloroform liquid membrane, into a receiving phase with pH 12, with efficiencies over 90%. 相似文献
33.
Frans M. van der Kloet Margriet Hendriks Thomas Hankemeier Theo Reijmers 《Analytica chimica acta》2013
Because of its high sensitivity and specificity, hyphenated mass spectrometry has become the predominant method to detect and quantify metabolites present in bio-samples relevant for all sorts of life science studies being executed. In contrast to targeted methods that are dedicated to specific features, global profiling acquisition methods allow new unspecific metabolites to be analyzed. The challenge with these so-called untargeted methods is the proper and automated extraction and integration of features that could be of relevance. We propose a new algorithm that enables untargeted integration of samples that are measured with high resolution liquid chromatography–mass spectrometry (LC–MS). In contrast to other approaches limited user interaction is needed allowing also less experienced users to integrate their data. The large amount of single features that are found within a sample is combined to a smaller list of, compound-related, grouped feature-sets representative for that sample. These feature-sets allow for easier interpretation and identification and as important, easier matching over samples. We show that the automatic obtained integration results for a set of known target metabolites match those generated with vendor software but that at least 10 times more feature-sets are extracted as well. We demonstrate our approach using high resolution LC–MS data acquired for 128 samples on a lipidomics platform. The data was also processed in a targeted manner (with a combination of automatic and manual integration) using vendor software for a set of 174 targets. As our untargeted extraction procedure is run per sample and per mass trace the implementation of it is scalable. Because of the generic approach, we envision that this data extraction lipids method will be used in a targeted as well as untargeted analysis of many different kinds of TOF-MS data, even CE- and GC–MS data or MRM. The Matlab package is available for download on request and efforts are directed toward a user-friendly Windows executable. 相似文献
34.
Arthur K. Sumner Maitreyi Saha Jadu G. Saha 《International journal of environmental analytical chemistry》2013,93(2):139-147
Abstract Residues of Dyfonate-ring-14C were extracted from a clay loam soil with various solvents under a variety of conditions. Recovery of radioactivity from the soil was not related to the polarity (dipole moment) or the dielectric constant of the solvents. Commonly used solvents such as acetone, methanol, ethanol, and hexane/acetone (1:1) extracted only 28, 44, 27, and 25%, respectively, of the residues from the air-dried soil. The extraction efficiencies were increased to 46, 60, 54, and 49%, respectively, when 20% water was added to the soil prior to extraction with these solvents. The amount of water added to the soil and time of contact with water also affected the recovery of radioactivity from the soil. Any of the solvents or methods investigated failed to recover more than 60% of the radioactivity in the soil, indicating that residues of Dyfonate were strongly bound to the soil and were difficult to recover. 相似文献
35.
This article describes the preconcentration of methyl methacrylate in produced water by the dispersive liquid–liquid microextraction using extraction solvents lighter than water followed by gas chromatography. In the present experiments, 0.4 mL dispersive solvent (ethanol) containing 15.0 μL extraction solvent (toluene) was rapidly injected into the samples and followed by centrifuging and direct injection into the gas chromatograph equipped with flame ionization detector. The parameters affecting the extraction efficiency were evaluated and optimized including toluene (as extraction solvent), ethanol (as dispersive solvent), 15 μL and 0.4 mL (as the volume of extraction and dispersive solvents, respectively), pH 7, 20% ionic strength, and extraction's temperature and time of 20°C and 10 min, respectively. Under the optimum conditions, the figures of merits were determined to be LOD = 10 μg/L, dynamic range = 20–180 μg/L, RSD = 11% (n = 6). The maximum recovery under the optimized condition was determined to be 79.4%. 相似文献
36.
Sample preparation is always the major bottleneck in analytical chemistry for the determination of pesticide residues. Different sample preparation methods have been proposed due to the wide variety of pesticides used and the inherent complexity of the matrices. In this study, different sample preparation methods including SPE, matrix solid‐phase dispersion, the quick, easy, cheap, efficient, rugged, and safe method, and a one‐step completion method were compared and evaluated for extracting pesticides from lotus seeds. Analysis was carried out using GC with electron‐capture detection. The results showed that good recoveries for tested pesticides were obtained by using Florisil in the four methods, and the extraction efficiency of the one‐step completion method was superior to the other three methods. The one‐step completion method was confirmed to have good linearity, reproducibility, stability, and recovery for the detection of 36 pesticides in lotus seed samples. The data collected from this study are expected to prove useful in regulating the concentration of the residues in lotus seeds, as well as in protecting human health from the hazards posed by these residues. 相似文献
37.
The application of an extraction column model which takes into account the influence of the forward mixing model is brought forward by generation of values of the mass transfer and axial dispersion coefficients required by the model. Values of these coefficients were generated from solute concentration profile measurements in a rotary disc contactor (RDC). The use of the Handlos–Baron drop mass transfer model was justified. The resulting continuous phase transfer coefficients were found to be dependent largely on disc speed. The accuracy of the forward mixing model for kerosene–acetic acid–water system was adequately presented and explained by the axial dispersion coefficient. 相似文献
38.
Monitoring of estradiol and its metabolites in biological samples is essential for the accurate diagnosis of a number of endocrine diseases. In this study, a sensitive, precise and specific GC–MS/MS method for the quantification of 17β-estradiol (17-BE) and its main metabolite, 2-methoxyestradiol (2-MEOE), in plasma was developed and validated. Plasma concentrations of these steroids are currently investigated as diagnostic markers for pre-eclampsia, a systematic disorder of pregnancy and a leading cause of maternal and fetal morbidity and mortality worldwide. 相似文献
39.
40.
以正十二烷作稀释剂, 研究了二(2-乙基己基)二硫代次膦酸(D2EHDTPA)对HNO3溶液中Am3+和Eu3+的萃取行为. 考察了酸度、 萃取剂及N 浓度和皂化度对萃取的影响. 在考察的pH范围(2.5~4.5)内, D2EHDTPA萃取Am3+和Eu3+的分配比(D)随pH值增大而增加; pH=3.65时, 分离因子(SFAm/Eu)值达到最大(4000). 随D2EHDTPA浓度的增加, DAm和DEu值均增加. 斜率分析表明, D2EHDTPA萃取Am3+和Eu3+主要形成3:1和2:1型的萃合物. N 未直接参与D2EHDTPA对Am3+和Eu3+的萃取反应. D2EHDTPA经NaOH皂化后, 萃取能力显著增强, SFAm/Eu值提高到104量级, 萃取容量约为理论值的60%. 此外, 使用高分辨质谱、 红外光谱和等温微量热滴定方法研究了D2EHDTPA与Eu3+的配位化学行为, 得到了金属离子与配体的组成比、 络合物稳定常数以及配位热力学参数ΔH, ΔS和ΔG值. 相似文献