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1.
Several reviews have been published on high-performance liquid chromatographic (HPLC) methods for the determination of aminoglycoside antibiotics (aminoglycosides) in biological fluids [e.g. Nilsson-Ehle, I. (1983). J. Liq. Chromat. 6: 251]. Of these, the paper by Maitra et al. [(1979a). Clin. Chem. 25: 1361.] briefly summarizes the early 2-3 years of experience on HPLC assaying of amikacin, gentamicin, netilmicin and tobramycin in body fluids. The reviews by Nilsson-Ehle, I. [(1983). J. Liq. Chromat. 6: 251] and by Miner, D. J. [(1985). Antibiotics. In Therapeutic Drug Monitoring and Toxicology by Liquid Chromatography, (Wong S. H. Y., ed.), ch. 10, p. 269. Marcel Dekker, New York and Basel.] devoted to the monitoring of antibiotics, also evaluated the first 6-8 years of the application of HPLC assays for the aminoglycosides amikacin, gentamicin, netilmicin, sisomicin and tobramycin. This report presents a great majority of the HPLC assay methods published during the last two decades for determining practically a dozen different aminoglycoside antibiotics in body fluids, particularly in the serum or plasma, and in urine.  相似文献   

2.
3.
R F Duncan 《Electrophoresis》1990,11(3):219-227
Infection of tissue culture cells with certain viruses results in the shutoff of host cell protein synthesis. We have examined virally infected cell lysates using two-dimensional gel electrophoresis and immunoblotting to ascertain whether initiation factor protein modifications are correlated with translational repression. Moderate increases in eukaryotic initiation factor (eIF)-2 alpha phosphorylation are detected in reovirus- and adenovirus-infected cells, as reported previously (Samuel et al., 1984; O'Malley et al., 1989). Neither vesicular stomatitis virus, vaccinia virus, frog virus III, rhinovirus, nor encephalomyocarditis virus caused significantly increased 2 alpha phosphorylation. There were no reproducible, significant changes in eIF-4A, eIF-4B, or eIF-2 beta in cells infected by any of these viruses. The cleavage of eIF-4F subunit p220, such as has been previously demonstrated to occur in poliovirus (Etchison et al., 1982) and rhinovirus (Etchison and Fout, 1985), was not detected in any of the other virus infections analyzed.  相似文献   

4.
Sulphate conjugation of p-nitrophenol (p-NP) in the liver and platelet cytosol of guinea pigs, rabbits and dogs were studied. The dependency of phenol sulphotransferase (PST) activity on p-NP concentration in the liver of guinea pigs and rabbits and in the platelets of guinea pigs were similar to that reported for the liver (Mizuma et al., J. Pharmacobio-Dyn., 6, 851 (1983)) and platelets (Nakamura et al., J. Pharm. Pharmacol., 42, 207 (1990)) of rats. There was one peak of PST activity on p-NP at the concentration of 1 to 10 microM, and the PST activity was increased again with an increase of p-NP concentration above the original concentration. On the other hand, a peak in PST activity on p-NP at the concentration of 1 to 10 microM was not observed in the platelets of rabbits and dogs. These results indicated species and organ differences in PST activity on p-NP in liver and platelets. The biphasic activities of the PST and p-NP in platelets and liver of rat and guinea pig were similar to that reported in humans (Reiter et al., Naunyn-Schmiedeberg's Arch. Pharmacol., 324, 140 (1983)).  相似文献   

5.
The direct correlation function of the complex discrete potential model fluids is obtained as a linear combination of the first-order mean spherical approximation (FMSA) solution for the simple square well model that has been reported recently [Hlushak et al., J. Chem. Phys. 130, 234511 (2009)]. The theory is employed to evaluate the structure and thermodynamics of complex fluids based on the square well-barrier and square well-barrier-well discrete potential models. Obtained results are compared with theoretical predictions of the hybrid mean spherical approximation, already reported in the literature [Guillen-Escamilla et al., J. Phys.: Condens. Matter 19, 086224 (2007)], and with computer simulation data of this study. The compressibility route to thermodynamics is then used to check whether the FMSA theory is able to predict multiple fluid-fluid transitions for the square barrier-well model fluids.  相似文献   

6.
State-of-the-art methods of the extraction, preconcentration, and determination of quercetin and other flavonoids are described. Different methods of sample preparation of real samples are compared, including solvent extraction from solid matrices and liquid-liquid, supercritical fluid, and solid-phase extraction. The following main determination methods are discussed: HPLC, thin-layer chromatography, capillary electrophoresis, spectrophotometry, luminescence, and electrochemical methods. Some examples of quercetin determination in biological fluids, food products, biologically active food supplements, pharmaceutical preparations, and plant samples are given.  相似文献   

7.
Two methods have been used to isolate Hb F from red cells with low levels of Hb F (less than 2% FAD), namely an alkali denaturation procedure, as described by Tsuchiya et al. [Dokkyo J. Med. Sci., 10 (1983) 13], and anion-exchange chromatography. Analyses of these Hb F enriched hemoglobin solutions by high-performance liquid chromatography allowed quantitation of the different gamma chains in the Hb F. Although the data showed considerable variation, particularly for samples with low levels of Hb F, the final results obtained with the two approaches were comparable, suggesting that the much simpler and more economical alkali denaturation procedure can be used for this purpose.  相似文献   

8.
The enhancement of the spin-lattice relaxation rate for nuclear spins in a ligand bound to a paramagnetic metal ion [known as the paramagnetic relaxation enhancement (PRE)] arises primarily through the dipole-dipole (DD) interaction between the nuclear spins and the electron spins. In solution, the DD interaction is modulated mostly by reorientation of the nuclear spin-electron spin axis and by electron spin relaxation. Calculations of the PRE are in general complicated, mainly because the electron spin interacts so strongly with the other degrees of freedom that its relaxation cannot be described by second-order perturbation theory or the Redfield theory. Three approaches to resolve this problem exist in the literature: The so-called slow-motion theory, originating from Swedish groups [Benetis et al., Mol. Phys. 48, 329 (1983); Kowalewski et al., Adv. Inorg. Chem. 57, (2005); Larsson et al., J. Chem. Phys. 101, 1116 (1994); T. Nilsson et al., J. Magn. Reson. 154, 269 (2002)] and two different methods based on simulations of the dynamics of electron spin in time domain, developed in Grenoble [Fries and Belorizky, J. Chem. Phys. 126, 204503 (2007); Rast et al., ibid. 115, 7554 (2001)] and Ann Arbor [Abernathy and Sharp, J. Chem. Phys. 106, 9032 (1997); Schaefle and Sharp, ibid. 121, 5387 (2004); Schaefle and Sharp, J. Magn. Reson. 176, 160 (2005)], respectively. In this paper, we report a numerical comparison of the three methods for a large variety of parameter sets, meant to correspond to large and small complexes of gadolinium(III) and of nickel(II). It is found that the agreement between the Swedish and the Grenoble approaches is very good for practically all parameter sets, while the predictions of the Ann Arbor model are similar in a number of the calculations but deviate significantly in others, reflecting in part differences in the treatment of electron spin relaxation. The origins of the discrepancies are discussed briefly.  相似文献   

9.
Ivory CF 《Electrophoresis》2007,28(1-2):15-25
The segregation and analysis of low-abundance proteins from complex biological fluids requires serial application of separation techniques that can simultaneously fractionate and concentrate solutes. In general, these techniques belong either to the family of displacement methods, e.g., ITP, or to the gradient methods, e.g., gradient-elution HPLC. IEF is a member of the subset of the gradient methods referred to as equilibrium gradient methods (EGM) and has the important property that, starting from an arbitrarily distributed initial state, evolves over time to a self-sharpening, stationary steady state. Until the introduction of counteracting chromatographic electrophoresis by O'Farrell in 1985, IEF was the only known electrokinetic technique with this property. Today, the sub-family of electrokinetic EGMs has at least half a dozen members and is slowly growing. This review describes some of the essential properties of the displacement methods, the EGMs and the non-EGMs, showing how they can be applied in microelectromechanical systems platforms, how their performance can be predicted and how new members with orthogonal properties may be added to the EGM family.  相似文献   

10.
A highly sensitive method for the determination of cholesterol in biological fluids is described. Unsaponifiable lipids from rat serum and thoracic duct lymph chylomicron samples were treated with cholesterol oxidase. The product of the enzymatic reaction, delta 4-cholestenone, was analysed by normal-phase high-performance liquid chromatography (HPLC) using hexane-isopropanol (95:5, v/v) as a mobile phase and detected with a UV spectrophotometer at 240 nm. When the standard samples containing varying amounts of cholesterol (0.15-3 nmol) were treated with cholesterol oxidase and analysed by HPLC (injected amounts 0.09-1.8 nmol of cholesterol), the peak areas increased proportionally with the amounts of authentic cholesterol with a correlation coefficient of 0.996. The values in these biological fluids determined by the HPLC method were identical to those obtained by enzymatic-colorimetric or gas chromatographic methods. Moreover, the detection limit (0.09 nmol) of the present method (0.15 nmol are required for the sample preparation) is lower than those of conventional methods (approximately 30 nmol). Because of the excellent sensitivity and reproducibility, this method is well suited for the determination of cholesterol in biological fluids where cholesterol concentration is low.  相似文献   

11.
《Analytical letters》2012,45(9-10):1065-1081
Abstract

A reversed phase high-performance liquid chromatographic (HPLC) method has been established for the separation and quantitative determination of the alkaloid codeine in pharmaceutical preparations and in body fluids. The minimum detectable concentrations for body fluids were 5ppb and 7ppb respectively for urine and whole blood with an analysis time of under 5 min. A RP-8 Spheri-5 guard column and a RP-8 Lichrosorb-10 column were used and codeine was detected at its absorption maximum wavelength of 212 nm using an eluting system of methanol: 0.5% w/v aqueous ammonium acetate (70:30) at a pH of about 7.0.  相似文献   

12.
Book Reviews     
Abstract

WATER AND WATER ANALYSIS (in German: Wasser und Wasseruntersuchung), 2nd revised edition in the Series “Laboratory Books in Chemistry”, by Leonhard A. Hiitter, A-6060 Hall in Tirol, Austria, 344 pages (including 38 figures, 34 tables, 43 pages with newest literature references and other informations (regulations, addresses) mainly from Germany, Austria and Switzerland, and a good index of nine pages), carton cover, format 227 × 165 mm, ISBN 3-425-05075-3, Verlag Diesterweg/Salle, D-6000 Frankfurt/Main and Sauerlander, CH-5000 Aarau (1984), DM 48.00

AQUATIC TOXICOLOGY, Volume 2 of a Series, edited by Laverne J. Weber, Marine Science Center, Oregon State University, Newport, Oregon, U.S.A., 236 pages (including 7 tables, 33 figures, references (mainly of the 1970's) added to each chapter, and a valuable subject index of 6 pages), linen, format 243 × 163 mm, ISBN 0-89004-439-2, Raven Press, New York 10036 (1984), US $55.00

TOXICITY TESTING, NEW APPROACHES AND APPLICATIONS IN HUMAN RISK ASSESSMENT, edited by Dr. A. P. Li et al., Enviromental Health Laboratory Monsanto Company, St. Louis, Missouri, U.S.A., 295 pages (including 37 tables, 49 figures, newest references added to each contribution, discussion statements, a good subject index of six pages, and an address list of contributors), linen, format 241 × 162mm, ISBN 0-88167-083-9, Raven Press, New York (1983/1985), US $50.50

HEALTH RISKS TO FEMALE WORKERS IN OCCUPATIONAL EXPOSURE TO CHEMICAL AGENTS, by Prof. Dr. Reinier L. Zielhuis et al., Coronel Laboratorium, Universiteit van NL-1054 BW Amsterdam, The Netherlands, 132 pages (including 30 tables, references added to each chapter, an appendix on recent data, but no subject index), soft cover, format 242 × 165mm, ISBN 3-540- 13579-0, Springer-Verlag, Berlin-Heidelberg-New York-Tokyo (1984), DM 70.00, or approximately US $24.60

IS THE SOIL DYING (in German: Stirbt der Boden)? GDI-Series Man-Nature-Environment, by Dr. Volker Hauff et al., D-5300 Bonn, 250 pages (including 49 figures, 34 tables, an author index of two pages, but no subject index), soft cover, format 241 × 171 mm, no ISBN-number, GDI-Buchhandlung, CH-8803 Riischlikon, Switzerland (1985), SFr. 50.00

THE HANDBOOK OF ENVIRONMENTAL CHEMISTRY, PARTS C and D, edited by Prof. Dr. Otto Hutzinger, Chair of Ecological Chemistry and Geochemistry, D-8580 Bayreuth, linen, format 248 × 170 mm, Springer-Verlag Berlin-Heidelberg-New York-Tokyo (1985).  相似文献   

13.
Summary We introduce an approach by which novel ligands can be designed for a receptor if a pharmacophore geometry has been established and the receptor-bound conformations of other ligands are known. We use the shape-matching method of Kuntz et al. [J. Mol. Biol., 161 (1982) 269–288] to search a database of molecular shapes for those molecules which can fit inside the combined volume of the known ligands and which have interatomic distances compatible with the pharmacophore geometry. Some of these molecules are then modified by interactive modeling techniques to better match the chemical properties of the known ligands. Our shape database (about 5000 candidate molecules) is derived from a subset of the Cambridge Crystallographic Database [Allen et al., Acta Crystallogr., Sect. B,35 (1979) 2331–2339]. We show, as an example, how several novel designs for nicotinic agonists can be derived by this approach, given a pharmacophore model derived from known agonists [Sheridan et al., J. Med. Chem., 29 (1986) 889–906]. This report complements our previous report [DesJarlais et al., J. Med. Chem., in press], which introduced a similar method for designing ligands when the structure of the receptor is known.  相似文献   

14.
Sanbe H  Haginaka J 《The Analyst》2003,128(6):593-597
A restricted access media-molecularly imprinted polymer (RAM-MIP) for propranolol (PRP) has been prepared for direct injection analysis of beta-blockers in biological fluids. First, the MIP for PRP was prepared using methacrylic acid and ethylene glycol dimethacrylate as the functional monomer and cross-linker, respectively, by a multi-step swelling and polymerization method. Next, a 1:1 mixture of glycerol monomethacrylate and glycerol dimethacrylate was used for hydrophilic surface modification, and added directly to the MIP for PRP after 4 h from the start of polymerization. Then further polymerization was carried out for 20 h. The obtained RAM-MIP for PRP showed excellent molecular recognition ability for PRP, good ones for alprenolol (ALP) and pindolol, and fair ones for other beta-blockers. The RAM-MIP was applied for direct injection analysis of ALP enantiomers in a rat plasma sample by a column-switching HPLC system using a beta-cyclodextrin phenylcarbamate-bonded silica column as the analytical column. The calibration graph, constructed from peak area versus each ALP enantiomer concentration, was linear with a correlation coefficient of > 0.999 over the concentration ranges of 12.5-250 ng ml(-1). The limit of quantitation was 12.5 ng ml(-1) with a 50 microl injection. This method could be applicable for the assay of ALP enantiomers at the therapeutic plasma levels, and have wide applicability for the assay of beta-blockers in biological fluids.  相似文献   

15.
Simultaneous Determination of Vitamins.--Klejdus et al. described a simultaneous determination of 10 water- and 10 fat-soluble vitamins in pharmaceutical preparations by liquid chromatography-diode-array detection (LC-DAD). A combined isocratic and linear gradient allowed separation of vitamins in 3 distinct groups: polar, low-polar, and nonpolar. The method was applied to pharmaceutical preparations, fortified powdered drinks, and food samples, for which results were in good agreement with values claimed. Heudi et al. described a separation of 9 water-soluble vitamins by LC-UV. The method was applied for the quantification of vitamins in polyvitaminated premixes used for the fortification of infant nutrition products. The repeatability of the method was evaluated at different concentration levels and coefficients of variation were <6.5%. The concentrations of vitamins found in premixes with the method were comparable to the values declared. A disadvantage of the methods mentioned above is that sample composition has to be known in advance. According to European legislation, for example, foods might be fortified with riboflavin phosphate or thiamin phosphate, vitamers which are not included in the simultaneous separations described. Vitamin B2.--Vi?as et al. elaborated an LC analysis of riboflavin vitamers in foods. Vitamin B2 can be found in nature as the free riboflavin, but in most biological materials it occurs predominantly in the form of 2 coenzymes, flavin mononucleotide (FMN) and flavin-adenine dinucleotide (FAD). Several methods usually involve the conversion of these coenzymes into free riboflavin before quantification of total riboflavin. According to the authors, there is growing interest to know flavin composition of foods. The described method separates the individual vitamers isocratically. Accuracy of the method is tested with 2 certified reference materials (CRMs). Vitamin B5.-Methods for the determination of vitamin B5 in foods are limited because of their low sensitivity and poor selectivity. Pakin et al. proposed a post-column derivatization of pantothenic acid as a fluorescent compound and used this principle in a specific and sensitive method for the determination of free and bound pantothenic acid in a large variety of foods. A French laboratory invited European laboratories to participate in a series of collaborative studies for this method, which will be carried out in 2005/2006. A more sophisticated method was described by Mittermayer et al. They developed an LC-mass spectrometry (LC/MS) method for the determination of vitamin B5 in a wide range of fortified food products. Application of the method to various samples showed consistent results with those obtained by microbiology. Vitamin B6.-Method 2004.07, an LC method for the analysis of vitamin B6 in reconstituted infant formula, was published by Mann et al. In contrast with this method, which quantifies vitamin B6 after converting the phosphorylated and free vitamers into pyridoxine, Vi?as et al. published an LC method which determines 6 vitamin B6 related compounds, the 3 B6 vitamers, their corresponding phosphorylated esters, and a metabolite. Accuracy was determined using 2 CRMs. Results were within the certified ranges. Vitamin C.-Franke et al. described an extensive study to vitamin C and flavonoid levels of fruits and vegetables consumed in Hawaii. Vitamin C was determined by measuring ascorbic acid in its reduced state by LC and coulometric detection along with UV absorbance detection at 245 nm. No attempts were made to assess levels of dehydroascorbic acid. Most recent research revealed that cell uptake of dehydroascorbic acid is unlikely to play a major role, which may explain the very low vitamin C activity of orally administered L-dehydroascorbic acid in rats. The food levels found by Franke et al. are variably lower, higher, or equal in comparison to other studies. Iwase described a method for the determination of ascorbic acid in foods using L-methionine for the pre-analysis sample stabilization. Electrochemical detection was used for the quantification. Traditionally, metaphosphoric acid was proven to be a useful dissolving agent for the determination of ascorbic acid. However, it dissolves in water very slowly, it is hygroscopic, and accurate weighing is not easy. Adjustment at pH 2-3 takes a long time. It appeared to be possible to replace metaphosphoric acid by 0.2% phosphoric acid. Methionine played an important role on the stability of ascorbic acid. The method seemed to be applicable to the routine analysis of ascorbic acid in foods. Folic Acid.-Microbiological analysis of total folate in foods is often considered as the golden standard compared to other methods based on, for example, LC. Koontz et al. showed results of total folate concentrations measured by microbiological assay in a variety of foods. Samples were submitted in a routine manner to experienced laboratories that regularly perform folate analysis fee-for-service basis in the United States. Each laboratory reported the use of a microbiological method similar to the AOAC Official Method for the determination of folic acid. Striking was, the use of 3 different pH extraction conditions by 4 laboratories. Only one laboratory reported using a tri-enzyme extraction. Results were evaluated. Results for folic acid fortified foods had considerably lower between-laboratory variation, 9-11%, versus >45% for other foods. Mean total folate ranged from 14 to 279 microg/100 g for a mixed vegetable reference material, from 5 to 70 microg/100 g for strawberries, and from 28 to 81 microg/100 g for wholemeal flour. One should realize a large variation in results, which might be caused by slight modifications in the microbiological analysis of total folate in foods or the analysis in various (unfortified) food matrixes. Furthermore, optimal combination of enzymes and reaction conditions may vary depending on the composition of the food. Padrangi and Laborde showed recently that treatment with alpha-amylase had no significant effect on measured folate in spinach, although addition of protease significantly increased the release of folate. LC/MS applications gain increasing attention because of their specificity. Rychlik used stable isotope dilution assays for the determination of the folate content of broccoli and bread. Compared to data in the literature and food data bases, amounts were significantly lower. Pawlosky et al., however, found comparable values for 5-methyltetrahydrofolic acid and folic acid by HPLC analysis with fluorescent detection and HPLC/MS. Among samples analyzed were CRMs and broccoli. Besides folic acid, other water-soluble vitamins were also determined by LC/MS/MS by Leporati et al. The method was applied to the quantitative analysis of the natural content of vitamins in typical Italian pasta samples, as well as in fortified pasta samples produced for the U.S. market. Biotin.-A paper from Staggs et al. included the assertion that existing biotin data in food composition tables are inaccurate because the majority are based on bioassays with all relevant disadvantages. Data in most cases are overestimated with consequences for recommendations for dietary biotin intake. An HPLC/avidin-binding assay was used to analyze 87 foods to support the hypothesis mentioned.  相似文献   

16.
Mehta AC 《Talanta》1984,31(1):1-8
In recent years the need for rapid, sensitive and specific assays for benzodiazepines has resulted in the publication of a number of high-pressure liquid chromatographic (HPLC) methods for their determination. This paper reviews the methods available to date for the determination of chlordiazepoxide, clonazepam, diazepam, flurazepam, lorazepam, nitrazepam, oxazepam and their metabolites in biological fluids.  相似文献   

17.
Chromatographic analyses play an important role in the identification and determination of phase I and phase II drug metabolites. While the chemical standards of phase I metabolites are usually available from commercial sources or by various synthetic, degradation or isolation methods, the phase II drug metabolites have usually more complicated structures, their standards are in general inaccessible and their identification and determination require a comprehensive analytical approach involving the use of xenobiochemical methods and the employment of hyphenated analytical techniques. In this work, various high-performance liquid chromatography (HPLC) methods were employed in the evaluation of xenobiochemical experiments leading to the identification and determination of phase II nabumetone metabolites. Optimal conditions for the quantitative enzymatic deconjugation of phase II metabolites were found for the samples of minipig bile, small intestine contents and urine. Comparative HPLC analyses of the samples of above-mentioned biomatrices and of the same biomatrices after their enzymatic treatment using beta-glucuronidase and arylsulfatase afforded the qualitative and quantitative information about phase II nabumetone metabolites. Hereby, three principal phase II nabumetone metabolites (ether glucuronides) were discovered in minipig's body fluids and their structures were confirmed using liquid chromatography (LC)-electrospray ionization mass spectrometric (MS) analyses.  相似文献   

18.
The recent mapping of the human genome was a tremendous achievement made possible to a large degree by the development of analytical methods for sequencing purine and pyrimidine bases in nucleic acids. In the last 3 decades, the number of analyses of nucleic acids and their constituents by HPLC and capillary electrophoresis (CE) has exploded. These techniques have been used not only for genomics, but also for the determination of free nucleotides, nucleosides and their bases in body fluids and tissues. Although a large number of HPLC and CE papers have been published on nucleic acid constituent applications, relatively little has been written on the mechanisms of the separations. However, to optimize analytical conditions knowledgeably and rapidly, it is important to know why and how these separations occur and the factors that affect them. The HPLC methods for the analysis of nucleic acid constituents and the information available on some of the mechanisms of separation of nucleotides, nucleosides and their bases, as well as the analysis of these compounds by CE and the factors that affect these separations are discussed.  相似文献   

19.
A. Aszalos 《Chromatographia》1985,20(5):313-322
Summary The use of high-performance liquid chromatography (HPLC) for the identification and determination of tetracycline antibiotics is reviewed. HPLC chromatograms provide fast identification by retention time, tR, and precise quantitation by measurement of peak height or peak area. For separation of tetracycline compounds, most HPLC methods use reversed-phase C18 or C8 columns and UV detection. The HPLC solvent system should have a pH of about 6 to prevent steric changes in the tetracycline molecule. For accurate quantitation it is necessary to avoid tailing and this is accomplished by adding a zwitter ion to the solvent system. Methanol and acetonitrile are frequently used as organic modifiers in these solvent systems. In a single analysis, HPLC methods can be used to separate as many as nine or ten commercially used tetracycline compounds and to determine four to five tetracyclines in commercial tetracycline preparations or in biological fluids.  相似文献   

20.
The aim of the present work is to show that spectroscopic and ultrasonic methods are powerful in situ methods for monitoring polymerization processes and for the determination of the composition of polymer blends and additives during extrusion. Quantitative analysis carried out with chemometric methods can determine the composition of multicomponent polymer mixtures and predict real world samples in real-time during extrusion. Examples are the modification of hyperbranched poly(urea-urethane)s, the polymerization of MMA, the real-time determination of flame retardants in PA, and the determination of the composition of the blend PE/PS. To cite this article: D. Fischer et al., C. R. Chimie 9 (2006).  相似文献   

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