共查询到20条相似文献,搜索用时 15 毫秒
1.
The enantiomers of caderoflxacin (CS-940), the new antibacterial fluoroquinolone compound, were separated on the commercially available α-acid glycoprotein-coated chiral stationary phase (Chiral-AGP) using the mobile phase of IPA: 0.15 M NaH2PO4 + Et3N (pH 7.9) = 3: 97 at 0.8 mL/min with UV detection at 282 nm. The chromatographic behavior of caderofloxacin enantiomers was investigated by varying the mobile phase conditions. The chiral assay method was validated and used to determination of (R)-Caderofloxacin in (S)-Caderofloxacin raw material samples. 相似文献
2.
A computer-assisted method is described for optimization of multi-component,mobile phase selection for separation of five phosphoamidothioate enantiomers with a series of silica and chiral columns in normal phase HPLC.The method is based on the triangular solvent selection concept using a statistical scanning method.The optimization of the separation over the experimental region is based on a special polynomial estimation from seven experimental runs,and resolution (Rs) is used as the selection criterion.Excellent agreement was obtained between predicted and experimental data. 相似文献
3.
Akhmad Sabarudin Junchao Huang Shin Shu Shinnosuke Sakagawa Tomonari Umemura 《Analytica chimica acta》2012
In this paper, we report on the preparation of a microbore-scale (1 mm i.d.) anion-exchange monolithic column suitable not only for analytical purposes but also for potentially preparative applications. In order to meet the conflicting requirements of high permeability and good mechanical strength, the following two-step procedure was applied. First, an epoxy-containing monolith was synthesized by in situ copolymerization of glycidyl methacrylate (GMA) and ethylene dimethacrylate (EDMA) within the confines of a silicosteel tubing of 1.02 mm i.d. and 1/16″ o.d. in the presence of a ternary porogenic mixture of 1-propanol, 1,4-butanediol, and water. The monolithic matrix was subsequently converted into weak anion-exchanger via the ring-opening reaction of epoxy group with diethyl amine. The dynamic binding capacity was 21.4 mg mL−1 for bovine serum albumin (BSA) at 10% breakthrough. The morphology and porous structure of this monolith were assessed by scanning electron microscope (SEM) and inverse size exclusion chromatography (ISEC). To optimize the separation efficiency, the effects of various chromatographic parameters upon the separation of DNA fragments were investigated. The resulting monolithic anion exchanger demonstrated good potential for the separation of both single- and double-stranded DNA molecules using a gradient elution with NaCl in Tris–HCl buffer (20 mM). Oligodeoxythymidylic acids (dT12–dT18) were successfully resolved at pH 8, while the fragments of 20 bp DNA ladder, 100 bp DNA ladder, and pBR322-HaeIII digest were efficiently separated at pH 9. 相似文献
4.
《Electrophoresis》2017,38(24):3124-3129
The combination of capillaries with different internal diameters was used to accelerate the separation of enantiomers in capillary electrophoresis. Separation of R ,S‐1,1′‐binaphthalene‐2,2′‐diyl hydrogen phosphate using isopropyl derivative of cyclofructan 6 was studied as a model system. The best separation conditions included 500 mM sodium borate pH 9.5 with 60 mM concentration of the chiral selector. Separation lasted approx. 1.5 min using the combination of 50 and 100 μm id capillaries of 9.7 cm and 22.9 cm, respectively. It allowed approx. 12‐fold acceleration in comparison to the traditional long‐end separation mainly due to the higher electroosmotic flow generated in the connected capillaries. 相似文献
5.
Itoh S Kawasaki N Ohta M Hyuga M Hyuga S Hayakawa T 《Journal of chromatography. A》2002,968(1-2):89-100
We previously reported that graphitized carbon column liquid chromatography-mass spectrometry (GCC-LC-MS) is very useful for the structural analysis of carbohydrates in a glycoprotein. In this study, GCC-LC-MS was adapted for the simultaneous microanalysis of oligosaccharides. A variety of oligosaccharide alditols prepared from fetuin, ribonuclease B, and recombinant human erythropoietin were used as model oligosaccharides. The use of microbore GCC-LC-MS was found to be successful for rapid, sensitive, and simultaneous analysis of high-mannose-type, desialylated fucosyl complex-type, sialylated complex-type, and sialylated fucosyl complex-type oligosaccharide alditols. Furthermore, we demonstrate that this method is applicable to the analysis of carbohydrate heterogeneity in a glycoprotein that possesses diverse oligosaccharides. Microbore GCC-LC-MS was able to characterize high-mannose-type, hybrid-type, and complex-type oligosaccharides in tissue plasminogen activator produced from human melanoma cells in a single analysis. 相似文献
6.
Liquid chromatographic determination of the enantiomers of ibuprofen in plasma using a chiral AGP column 总被引:1,自引:0,他引:1
A reversed-phase high-performance liquid chromatographic method has been developed for the determination of the R- and S-enantiomers of ibuprofen. The enantiomers and the internal standard 4-pentylphenylacetic acid are extracted from plasma, separated and quantified on a Chiral-AGP column using ultraviolet detection. The simplicity, sensitivity and precision of the method makes it convenient for use in pharmacokinetic studies. 相似文献
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8.
Liquid chromatographic separation of enantiomers of beta-amino acids using a chiral stationary phase
O W Griffith E B Campbell W H Pirkle A Tsipouras M H Hyun 《Journal of chromatography. A》1986,362(3):345-352
The enantiomers of both alpha-substituted beta-alanines and beta-substituted beta-alanines may be chromatographically separated using silica-bonded chiral stationary phases derived from N-acetylated alpha-arylalkylamines. The amino acids are chromatographed as alkyl esters of N-3,5-dinitrobenzoyl derivatives; separability factors range from 1.11 to 1.65 for nine alpha-substituted beta-alanines and from 1.08 to 1.20 for nine beta-substituted beta-alanines. The enantiomers of beta-aminoisobutyrate and beta-leucine, chiral beta-amino acids occurring in animal tissues and physiological fluids, are among those resolved. The enantiomers of R,S-beta-aminoisobutyrate and several related alpha-alkyl-beta-alanines were prepared by chromatographic resolution of diastereomeric dipeptides. 相似文献
9.
A novel oil-in-water microemulsion incorporating the chiral surfactant dodecoxycarbonylvaline (DDCV) was used to achieve the rapid enantiomeric separation of pharmaceutical drugs by electrokinetic chromatography (EKC). Incorporation of DDCV into a microemulsion resulted in an elution range more than double that provided the micellar form of the surfactant aggregate. Interestingly, for the same compounds the enantioselectivity provided by the chiral DDCV microemulsions ranged from 1.06-1.30 for the neutral and cationic drugs, which was slightly higher than that provided by chiral DDCV micelles. The use of a low surface tension oil (ethyl acetate) permitted a much lower concentration of chiral surfactant to be employed; this, together with the use of a zwitterionic buffer (ACES) resulted in a very low conductivity microemulsion that allowed a higher separation voltage to be utilized, resulting in rapid enantiomeric separations (< 8 min.). Mobility matching of the buffer cation(s) was used to improve peak shape and efficiencies. In our limited survey of the phase diagram, the optimum composition of the microemulsion buffer was 1.0% (w/v) DDCV (30 mM), 0.5% (v/v) ethyl acetate, 1.2% (v/v) 1-butanol and 50 mM ACES buffer at pH 7. 相似文献
10.
The IsoPrime multicompartment electrolyzer, equipped with a series of isoelectric membranes with closely spaced pI values, was used for the first time for the preparative-scale separation of the enantiomers of dansyl phenylalanine with hydroxypropyl beta-cyclodextrin as resolving agent. The final separation conditions could be established easily in three successive experiments by rationally narrowing the pH steps between the neighboring isoelectric membranes. The final separation yielded products with an enantiomeric excess greater than 99.9%, at production rates of about 0.1 mg/h. The greatest experimental difficulty was caused by the relatively high salt content of the hydroxypropyl beta-cyclodextrin used, which resulted in high conductivity and limited the maximum field strength one could use. 相似文献
11.
We developed a method to separate colloidally dispersed nanoparticles on monolithic capillary columns. Silica nanoparticles were eluted according to their sizes, and the plots of the logarithm of the size of nanoparticles against their elution volume showed good linearity (r=0.992) over wide range of sizes. Because of the high porosity of the monolithic column (porosity; 88%), the column's length could be increased without clogging of the dispersed samples and the pressure in a long column (500 mm × 0.2 mm i.d.) was low, with a value of 5.8 MPa at a flow rate of 1 μL/min. We demonstrate that this method using monolithic capillary columns could be used as a powerful tool for size separation of nanometer-size materials, which will open a new pathway to quality control of nanomaterials in nanotechnology applications. 相似文献
12.
The separation of bupropion enantiomers on an ovomucoid stationary phase was investigated. The mobile- and stationary-phase parameters that may influence the separation were identified. The parameters that were studied include: type and concentration of organic modifier, mobile phase pH, ionic strength, type of buffer, and column temperature, as well as the effect that the amount of sample injected had on the separation. The optimized chiral separation baseline-resolved the enantiomers in less than 10 min. Calibration curves for a standard were linear over a range of 0.27-53.0 microg/g (ppm) with a correlation coefficient of 0.999 for both enantiomers. A detection limit of 0.13 microg/g and a quantitation limit of 0.27 microg/g were also found. The system precision of the method was 0.2%. 相似文献
13.
A simple and highly sensitive method has been developed for determining ortho-phenylphenol (OPP) in lemon rind by high-performance liquid chromatography with electrochemical detection using a microbore column (microHPLC-ECD). Based on the voltammetric behavior of OPP, microHPLC-ECD was established using a CAPCELL PAK C-18 UG 120 microbore ODS column, 17 mM acetic acid-sodium acetate buffer (pH 4.0)/acetonitrile (60/40, v/v) as a mobile phase and an applied potential at +0.9 V vs. Ag/AgCl. The current peak height was found to be linearly related to the amount of OPP injected from 3.4 pg to 1.7 ng (r > 0.999). The detection limit (S/N = 3) was 3.4 pg (20 fmol), which was 100 times greater in terms of sensitivity when compared to conventional HPLC with UV detection. Standard OPP at 0.425 ng was detected with a relative standard deviation (RSD) of 1.9% (n = 10). The OPP contents in several lemon samples were determined by the present method. The recoveries of OPP from lemon rind exceeded 98% with an RSD (n = 5) of less than 3.01%. 相似文献
14.
《Trends in analytical chemistry : TRAC》1988,7(6):209-217
Addition of an optically active compound to the mobile phase is an attractive method for resolving enantiomers in liquid chromatography. The technique is practical, easy to use and allows rapid screening for new chiral complexing agents as well as for optimal separation conditions. 相似文献
15.
Silica gel thin-layer chromatography plates impregnated with macrocyclic antibiotic, vancomycin, as chiral selector were prepared and used for the resolution of (+/-)-verapamil. A mobile phase system of acetonitrile-methanol-water (15:2.5:2.5, v/v) was worked out systematically. The effects of chiral selector, temperature and pH on resolution were also studied. The spots were detected with iodine vapors and the detection limit was found to be 0.074 microg of each enantiomers. 相似文献
16.
Eva-Henrietta Dulf Cristina I. Muresan Mihaela L. Unguresan 《Journal of mathematical chemistry》2014,52(1):115-131
The chemical processes developed in the $^{15}$ N-isotope separation plant are very complex and many details are not yet known in totality. Accurate models for such isotope separation plants offer an invaluable insight towards optimizing the production and establishing an adequate control action. A model of such an isotope plant is presented in the paper. The results are validated by simulation, based on a lot of experiments. The model is then used to evaluate and establish the necessary conditions for a maximum production for an existing pilot plant. For protection purposes, the experimental data used in this paper have been scaled. 相似文献
17.
Kimura H Tanigawa T Morisaka H Ikegami T Hosoya K Ishizuka N Minakuchi H Nakanishi K Ueda M Cabrera K Tanaka N 《Journal of separation science》2004,27(10-11):897-904
Separation of peptides by fast and simple two-dimensional (2D)-HPLC was studied using a monolithic silica column as a second-dimension (2nd-D) column. Every fraction from the first column, 5 cm long (2.1 mm ID) packed with polymer-based cation exchange beads, was subjected to separation in the 2nd-D using an octadecylsilylated (C18) monolithic sillica column (4.6 mm ID, 2.5 cm). A capillary-type monolithic silica C18column (0.1 mm ID, 10 cm) was also employed as a 2nd-D column with split flow/injection. Effluentof the first dimension (1st-D) was directly loaded into an injector loop of 2nd-D HPLC. UV and MS detection were successfully carried out at high linear velocity of mobile phase at 2nd-D using flow splitting for the 4.6 mm ID 2nd-D column, or with directconnection of the capillary column to the MS interface. Two-minute fractionation inthe 1st-D, 118-second loading, and 2-second injection by the 2nd-D injector, allowed one minute for gradient separation in the 2nd-D, resulting in a maximum peak capacity of about 700 within 40 min. The use of a capillary column in solvent consumption and better MS detectability compared to a larger-sized column. This kind of fast and simple 2D-HPLC utilizing monolithic silica columns will be useful for the separation of complex mixtures in a short time. 相似文献
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19.
D. M. Musatov V. S. Kublitskii O. R. Malyshev D. V. Kurilov M. G. Vinogradov 《Russian Journal of Organic Chemistry》2007,43(12):1813-1814
Tetrahydrofurfurylamine enantiomers were separated on a preparative scale by fractional crystallization of diastereoisomeric salts with natural L-tartaric acid. (R)-Tetrahydrofurfurylamine was isolated in 68% yield with an optical purity of more than 98.5% according to the HPLC data. 相似文献