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  • 1
    Keywords: DRUG ; HPLC ; ASSAY ; CARCINOMA CELLS ; TANDEM MASS-SPECTROMETRY ; PURIFICATION ; LIQUID-CHROMATOGRAPHY ; 10-deacetylbaccatin III ; CULTURES ; HIMALAYAN YEW ; PACLITAXEL TAXOL ; PFP column ; taxoids ; Taxus ; WALLICHIANA
    Abstract: A simple and accurate RP-HPLC method with pentafluorophenyl (PFP) column was developed for the simultaneous determination of six taxoids, i.e. paclitaxel, 10-deacetylbaccatin III (10-DAB III), 7-xylosyl-10-deacetyltaxol (7-xyl-10-DAT), 10-deacetyltaxol (10-DAT), cephalomannine and 7-epi-10-deacetyltaxol (7-epi-10-DAT), In the extracts from the needles of three Taxus species. The mobile phase consisted of acetonitrile (A) and water (B), and the extracts were separated using gradient elution program: 30% A at the first 7 min, and then ramped to 42% A at 8 min, held until 38 min. The developed method was validated with satisfactory precision (RSD 〈 2.61%), repeatability (RSD 〈 2.92%) and recovery (95.19-104.47%). The above taxoids in the extracts of Tamus cuspidata, T. chinensis and T. media were analyzed with the developed RP-HPLC method, and the results showed that the contents of different taxoids in three mentioned species were distinct. Maximal amounts of 10-DAB III, 7-xyl-10-DAT and 7-epi-10-DAT appeared in T. chinensis, while T. media possessed the highest content of 10-DAT, cephalomannine and paclitaxel. The developed method is accurate and efficient. It can be reliably used in the improved determination of taxoids for the quality control of Taxus species. Copyright (c) 2008 John Wiley & Sons, Ltd
    Type of Publication: Journal article published
    PubMed ID: 18816506
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  • 2
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 1 (1986), S. 173-176 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: We describe an optimized automated liquid Chromatographic method for simultaneous measurement of primidone, phenobarbitone, phenytoin, carbamazepine and clonazepam. A Waters Tri-Module automation system is used and it provides direct read-out of results after chromatography. A one-step extraction with ethyl acetate is used to extract the drugs from 100 μL serum samples. We use an isocratic mobile phase and monitor the column effluent at 210 nm. Drug levels as low as 5 μmol/L can be detected. The within-run CV's range from 1.4 to 2.7%, and the between-run CV's range from 5.2 to 6.1%. Analytical recovery is in the range from 94-108%. The method compares favourably with the enzyme multiple immunoassay technique for routine antiepileptic drugs monitoring, in accuracy, efficiency and cost-effectiveness.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 3
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Rapid, quantitative, chromatographic separations of mixtures of human haemoglobins have been performed on short (5 - 20 mm) columns of packing material. The desirable characteristics of suitable column packing materials are illustrated and discussed. Simple, inexpensive, manually operated equipment can be used for the analysis, since the specifically designed midget columns generate little back pressure (10 - 30 lb/in2) when eluted at constant flow rates up to 2 mL/min. Cation exchange Chromatography on bonded silicas has been used for the detection of pathological haemoglobinopathies. Separations similar to the HPLC procedures are possible with the correct selection of buffer composition. It also compares favourably with the methods in common clinical use employing electrophoresis on cellulose acetate. Both ion-exchange and affinity methods for the estimation of glycated haemoglobins have been developed and are compared.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
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  • 4
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A simple and highly sensitive method for the determination of free and total (free + conjugated) catecholamines (norepinephrine, epinephrine and dopamine) in human urine is described which employs HPLC with fluorescence detection. Conjugated catecholamines (sulfate form) are hydrolyzed by a sulfatase-mediated reaction to the corresponding free amines. After cation exchange chromatography on a Toyopak IC-SPS cartridge, catecholamines and isoproterenol (internal standard) in urine samples were converted into the corresponding fluorescent compounds by reaction with 1, 2-diphenylethylenediamine. These compounds were separated within 8 min on a reversed phase column with isocratic elution using a mixture of water, methanol and acetonitrile containing a Tris-hydrochloric acid buffer (pH 7.0). The detection limit for each catecholamine is ca 2 fmol per 100 μL injection volume.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 5
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A rapid and specific HPLC method for the simultaneous determination of gastrodin and its metabolite gastrodigenin (p-hydroxybenzyl alcohol) in rat plasma, bile, liver, urine and faeces is described. The separation was achieved by using a reversed phase column (YWG-C18) eluted with methanol-water (2.5:97.5 v/v). Phloroglucinolum was used as internal standard and the peaks were detected at UV 221 nm. The protein precipitation with ethanol was a very simple and rapid method for sample preparation. The gastrodin and gastrodigenin were quantitated by measuring the peak-height ratios. There was a linear concentration range of 10-320 μg/mL in the assay for both compounds. The coefficients of variation (within-day) for samples spiked with gastrodin and gastrodigenin were 2.94% and 3.08%, respectively. The method demonstrated a high specificity and was suitable for use in pharmacokinetic studies.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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  • 6
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 2 (1987), S. 34-37 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A simple HPLC method has been developed to measure the antiarrhythmic agent penticainide and its N-desalkyl metabolite in biological fluids. Solvent extraction of a small (200 μL) sample volume with direct analysis of the extract is used to measure the plasma and urinary concentrations of these compounds attained during chronic therapy, although a larger sample volume (1.0 mL) and prior concentration of the extract are required for single oral dose work. In each case chromatographic analysis is performed using a microparticulate (5 μm) silica column and methanolic ammonium perchlorate (10 mM, pH 6.7) as eluent with UV detection (260 nm). No endogenous sources of interference have been encountered and potential interference from other drugs is minimal.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 7
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Because of their narrow therapeutic ranges and differing patient tolerances, the monitoring of tricyclic antidepressants (TADs) commonly prescribed for control of endogenous depression is highly desirable for the satisfactory treatment of patients. The majority of methods for analysis of TADs require multiple extractions from plasma with organic solvents, accompanied by obligatory centrifugation steps. We describe a simple procedure for the rapid extraction of serum TADs, with high recovery of the analyte drugs. It involves sample preparation using Analytichem ‘BOND-ELUT’ C-2 reverse phase columns, and analysis by gas chromatography using a nitrogen-phosphorus detector. The method offers a quick, inexpensive and low-maintenance assay which is applicable to all the common tricyclic class drugs.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 8
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A rapid, specific and sensitive method using reversed phase HPLC for the simultaneous determination of clozapine and its two metabolites in serum and urine has been developed. The mobile phase was a mixture of 67% (v/v) methanol in water containing 0.4% tetramethylethylenediamine and 0.32% acetic acid (pH 5.5). The influence of methanol content, the pH of the mobile phase and the effect of adding alkylammonium ions as peak tailing reducer in the mobile phase have been investigated. The solvent for extracting clozapine from serum and urine was ether. 50 μ1 of 0.25 M H2SO4 solution was used to redissolve the dry residue to eliminate the endogenous compounds which could otherwise be eluted together with clozapine from the HPLC column. The analysis of a single sample was accomplished within half an hour. The identities of the chromatographic peaks of clozapine and its N-demethyl metabolite collected from the patient urine sample were confirmed by mass spectrometry. The method is sufficiently sensitive (5 ng/ml) and reproducible (CV 2.9%-6.7%) for clinical and pharmacokinetic studies, and preliminary results in these respects are presented.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
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  • 9
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Rapid sample preparation methods for the determination of sulfamethazine (SMZ) and its N4-acetyl and desamino metabolites in swine tissues at the 0.1 mg kg-1 level are presented. The methods use sonication-aided extraction with dichloromethane. For SMZ and N4-acetyl SMZ analysis extracts are cleaned up and concentrated on a silica disposable column followed by HPLC on a CP™ Spher C8 column using acetonitrile-sodium acetate buffer as the mobile phase. For desamino-SMZ analysis the extract was cleaned up and concentrated on a Florisil disposable column, followed by HPLC on a Nucleosil 5-CN column after formation of an ion-pair complex with 1-heptanesulfonic acid. For desamino SMZ peak identification by diode-array UV/VIS detection is also described. Mean recoveries from spiked tissue samples were about 87% (muscle) and 76% (kidney) for SMZ and N4-acetyl SMZ and about 70% for desamino SMZ.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 10
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Total opioid peptide receptoractivity in human cerebrospinal fluid is measured in patients who are experiencing lower back pain. Desalted CSF is eluted from a C18 Sep-Pak and is subjected to a radioreceptorassay (RRA) that employs tritiated etorphin, which is aligand that is effectively displaced by opioids from several different types of opioid receptors. Three clinical groups have significantly different endogenous levels of 2.4, 4.5, and 6.4 pmol of methionine enkephalin-equivalents per mL CSF. Those three levels indicate that more opioid activity is correlated with the amount of drug to relieve the patient's perception of pain. When the total opioid content exceeds an empirical threshold, the sample is further fractionated with gradient reversed phase HPLC, and the opioid receptoractivity in each HPLC fraction is measured to determine the characteristics pattern of those receptoractive opioid peptides present in that patient's CSF. Different HPLC RRA patterns are found for different clinical categories. A possible interpretation of these two different sets of data-is that a lesion exists in one or several of the opioid peptidergic systems (metabolism, receptors) in this particular patient population.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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