摘要:

AbstractChromatographic methods (paper chromatography, thin layer chromatography, high performance liquid chromatography, gas chromatography and gas chromatography‐mass spectrometry) for the determination of clinically important steroids in biological specimens are reviewed. The emphasis is on the use of gas chromatography, gas chromatography‐mass spectrometry and high performance liquid chromatography as reference rather than routine techniques. Chromatographic methods are compared with colorimetric, fluorimetric and radioimmunoassay procedures in terms of simplicity of operation, cost and ability to analyse large numbers of specimens. The importance of correct specimen collection and storage are discussed. Sample preparation techniques for the various analytical methods are described. These include extraction of free and conjugated steroids from serum, plasma, urine and saliva by solvent partition, with polymer‐based resins such as Amberlite XAD‐2, DEAE‐Sephadex and Sephadex resins bonded with various other function groups and, more recently, with chemically bonded reversed‐ph

ISSN:0269-3879    

DOI:10.1002/bmc.1130040102

出版商:John Wiley&Sons, Ltd.    

年代:1990

数据来源: WILEY

摘要:

AbstractA rapid sensitive and selective isocratic technique was developed for the analysis of plasma epirubicin and three of its known fluorescent metabolites epirubicinol, 4′‐O‐β‐D‐glucuronyl‐4′‐epidoxorubicin and 4′‐O‐β‐D‐glucuronyl 1,3‐dihydro‐4′‐epidoxorubicin, with daunorubicin as an internal standard, by using high performance liquid chromatography (HPLC) with fluorescence detection and a ‘Hypersil ODS’ column. The drugs were easily and efficiently extracted with a Sep‐Pak C18cartridge and the mean recoveries were greater than 85%. Intraassay and Interassay coefficients of variation (plasma samples) were better than 8.25%. An example of pharmacokinetic study obtained in a cancer patient after intraven

ISSN:0269-3879    

DOI:10.1002/bmc.1130040103

出版商:John Wiley&Sons, Ltd.    

年代:1990

数据来源: WILEY

摘要:

AbstractA fast and sensitive method is given for analysing urinary tryptophan and six of its metabolites on the nicotinic acid pathway. Kynurenine, tryptophan, 3‐hydroxykynurenine, anthranilic acid, 3‐hydroxyanthranilic acid, kynurenic acid and xanthurenic acid were isocratically eluted and completely resolved with a mobile phase of acetonitrile + sodium acetate buffer, pH 4.76 (4:96, v/v). The flow rate was 0.8 mL/min at the beginning and was then linearly increased to 1.2 after 6 min; after 14 min the flow was augmented from 1.2 to 2 mL/min. The effluent was monitored with a variable UV detector set at 254 nm for the first five peaks and at 280 and 325 nm for the penultimate peak and final peak. Analytical recoveries of the compounds after deproteinization varied between 64% and 98%. The reported method should enable one to examine easily, extensively, quantitatively and routinely urinary tryptophan and the most important metabolites of the nicotinic acid path

ISSN:0269-3879    

DOI:10.1002/bmc.1130040104

出版商:John Wiley&Sons, Ltd.    

年代:1990

数据来源: WILEY

摘要:

AbstractMidazolam concentrations in patients' plasma was determined after extraction with high performance liquid chromatography (HPLC), gas chromatography (GC) and gas chromatography/mass spectrometry (GC/MS). GC was selected for routine plasma assays in terms of selectivity, simplicity, precision, accuracy and sensitivity (0.02 μg/ml); HPLC analysis was less sensitive (0.1 μg/mL) than GC; GC/MS was used for analysis validation. Plasma protein binding of midazolam was determined by GC in patients' plasma after in vitro incubation with midazolam, ultrafiltration and extraction; 5% of the drug was unbound to plasma proteins. Midazolam distribution in lipoprotein fractions separated by ultracentrifugation of plasma obtained from patients on prolonged midazolam treatment was also assayed by G

ISSN:0269-3879    

DOI:10.1002/bmc.1130040105

出版商:John Wiley&Sons, Ltd.    

年代:1990

数据来源: WILEY

摘要:

AbstractAn optimization strategy for an isocratic reversed phase high performance liquid chromatographic system (RP‐HPLC) is described. Factorial design and a computer program are used to predict the retention time and resolution of fourteen steroids. An optimized rapid (<25 min) isocratic RP‐HPLC system for the satisfactory separation of cortisone, cortisol, corticosterone, 11‐deoxycortisol, 11‐deoxycorticosterone, 17α‐hydroxyprogesterone, progesterone, androstenedione, testosterone, estrone, estradiol, estriol, prednisone acetate and dexamethasone acetate has been developed using this strategy through eight e

ISSN:0269-3879    

DOI:10.1002/bmc.1130040106

出版商:John Wiley&Sons, Ltd.    

年代:1990

数据来源: WILEY

摘要:

AbstractReversed phase HPLC methodology has been developed for separation of peptide leukotrienes and indomethacin in porcine bile. Reproducible recoveries were obtained using radioactive leukotrienes ([3H]LTC4, 57.1 ± 2.5%; [3H]LTE4, 62.7 ± 1.9%; [3H]LTD4, 54.3 ± 2.7%). Radioimmunoassay of column eluant demonstrated that as little as 300 pg of exogenous leukotrienes could be measured in bile fluids, with similar recoveries. Analysis of bile sampled 60–90 min after initiation of experimental endotoxic shock in indomethacin treated pigs revealed a leukotriene concentration of 5.24 ± 1.16 ng/mL(LTD4). This was significantly greater (p<0.05,n= 3) than that observed in samples collected prior to endotoxin (0.42 ± 0.23 ng/mL), or from untreated animals (0.85 ± 0.51 ng/mL). This method is thus applicable to investigation of the role of 5‐lipoxygenase products in porcine models of human disease, including shock conditions such as endotoxaemia, during cyclooxygenase inhibition by ind

ISSN:0269-3879    

DOI:10.1002/bmc.1130040107

出版商:John Wiley&Sons, Ltd.    

年代:1990

数据来源: WILEY

摘要:

AbstractThe metabolités of lappaconitine in the urine of humans having been previously administered intramuscularly with lappaconitine hydrobromide were studied using high performance liquid chromatography with electrochemical and ultraviolet detection. The urine was extracted by means of liquid‐ and solid‐phase extractions. Each of the metabolites of lappaconitine was purified by high performance liquid chromatography on a reversed phase column and identified on the basis of the chromatographic behaviour and the detector response. It was proved that lappaconitine,N‐deacetyl‐16‐O‐demethyllappaconitine andN‐deacetyllappaconitine were excreted in urine from humans receiving

ISSN:0269-3879    

DOI:10.1002/bmc.1130040108

出版商:John Wiley&Sons, Ltd.    

年代:1990

数据来源: WILEY

ISSN:0269-3879    

DOI:10.1002/bmc.1130040110

出版商:John Wiley&Sons, Ltd.    

年代:1990

数据来源: WILEY