High-performance liquid chromatography of pyruvic and alpha-ketoglutaric acids and its application to urine samples.

1977 ◽  
Vol 23 (5) ◽  
pp. 802-805 ◽  
Author(s):  
J C Liao ◽  
N E Hoffman ◽  
J J Barboriak ◽  
D A Roth
Keyword(s):  
Aqueous Solution ◽  
High Performance Liquid Chromatography ◽  
High Performance ◽  
Ammonium Acetate ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Diabetic Patients ◽  
Reversed Phase Chromatography ◽  
Linear Gradient ◽  
Normal Individuals

Abstract Pyruvic and alpha-ketoglutaric acids were quantitatively and rapidly converted to quinoxalones by a new method, to enhance their detectability in the ultraviolet. The quinoxalones were separated by reversed-phase chromatography with use of 10 micronm particles packed in a 30-cm (length) column. An aqueous solution of ammonium acetate and methanol was used for linear gradient elution. The urinary excretion of pyruvic and alpha-ketoglutaric acids by normal individuals, diabetic patients, and patients with renal dysfunction was determined.

High Performance Liquid Chromatography Coupled with Radioactivity Detection: A Powerful Tool for Determining Drug Metabolite Profiles in Biological Fluids

1986 ◽  
Vol 41 (1-2) ◽  
pp. 115-125 ◽  
Author(s):  
K.-O. Vollmer ◽  
W. Klemisch ◽  
A. von Hodenberg
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Biological Fluids ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Isolation And Purification ◽  
Carbon 14 ◽  
Tracer Techniques ◽  
Metabolite Profiles

Abstract High performance liquid chromatography coupled with continuous radioactivity detection rep­resents an advancement in drug metabolism research. Using radioactive substances labelled in biologically stable positions, all metabolites can be specifically detected by radioactivity measure­ment. Thus no clean-up of biological fluids is required prior to HPLC. This can prevent artefact formation from unstable metabolites, reduces recovery problems and facilitates quantitation. Separation of highly polar and unpolar metabolites is possible in a single chromatographic run using gradient elution and reversed phase materials. This technique is also well-suited for prepara­tive isolation and purification of metabolites for subsequent structure elucidation. Various metabolite profiles of drugs labelled with carbon-14 or tritium are shown. Metabolites of the following drugs are presented: norfenefrine, etozolin, thymoxamine, naloxone, and levobunolol. We review the general methodology and report our experience with this technique. In principle, this technique may be useful for all biological systems in which tracer techniques are applied.

EVIDENCE FOR BIIIARY EXCRETION OF PHENPROCOUMON AND ITS METABOLITES IN HUMANS; IDENTIFICATION BY HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY AND GAS CHROMATOGRAPHY-MASS SPECTROMETRY

1987 ◽  
Author(s):  
J X de Vries ◽  
R Raedsch ◽  
A Stiehl ◽  
U Voelker ◽  
I Walter-Sack ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Gas Chromatography Mass Spectrometry ◽  
Phase Gradient ◽  
Chromatography Mass Spectrometry

Recently it has been shown that in man the oral couma-rin anticoagulant phenprocoumon is eliminated up to 60-70 % in urine and 30-40 % in faeces; in urine phenprocoumon (PH) and its metabolites 7-hydroxy-(7-OH),6-hydroxy-(6-OH) and 4'-hydroxy-(4'-OH) phenprocoumon are present mainly as conjugates. No data so far were available on the biliary excretion of these compounds.We examined bile obtained from four in-patients during PH treatment; bile samples were aspirated in the duodenum at the papilla during routine diagnostic endoscopy and immediately deep frozen before analysis. Samples were extracted both untreated as well as after hydrolysis with 6-glucuronidase/aryl sulfatase and separated by reversed phase gradient elution high performance liquid chromatography (HPLC) with fluorescence detection; for confirmation, the same extracts were methylated and analysed by gas chromatography-mass spectrometry (CG-MS) (J.X.de Vries et al J Chromatogr., 338 (1985) 325). PH, 7-OH, 6-OH and 4'-OH were identified by comparison with synthetic authentic samples'''''''

scholarly journals Separation of porphyrin isomers by high-performance liquid chromatography

1983 ◽  
Vol 211 (2) ◽  
pp. 435-438 ◽  
Author(s):  
C K Lim ◽  
J M Rideout ◽  
D J Wright
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Type I ◽  
Phase Gradient ◽  
Preparative Isolation ◽  
Type Iii ◽  
Simultaneous Separation

A reversed-phase gradient elution system is described for the simultaneous separation of the type I and type III isomers of 8-, 7-, 6-, 5- and 4-carboxylated porphyrins and isocoproporphyrins. The method, adaptable for isocratic and stepwise separation of individual groups of isomers, is also suitable for preparative isolation of pure porphyrins. The analyses of porphyrin isomers in the urine and faeces of porphyric patients are examples of applications.

Aqueous oxidation of acetaminophen with monochloramine

2017 ◽  
Vol 18 (5) ◽  
pp. 1769-1774
Author(s):  
O. Abou Mehrez ◽  
F. Masri ◽  
M. Baroudi ◽  
F. Dossier-Berne
Keyword(s):  
Aqueous Solution ◽  
High Performance Liquid Chromatography ◽  
High Performance ◽  
Order Rate Constant ◽  
Reversed Phase ◽  
Pain Reliever ◽  
Experimental Conditions ◽  
Ultraviolet Absorbance ◽  
The Common ◽  
Aqueous Oxidation

Abstract The reactivity of the common pain reliever acetaminophen (paracetamol or 4-acetamidophenol) with monochloramine in aqueous solution was investigated in this study. Initially, monochloramine demands of acetaminophen (AAP) and its chlorination byproduct, 1,4-benzoquinone, were determined in excess of oxidant at pH 8.5 and 25 °C. Monochloramine demands of AAP and 1,4-benzoquinone were respectively 1.2 (±0.2) and 4.4 (±0.3) mol/mol after 72 h of reaction. Chlorination reactions were also conducted under the same experimental conditions in order to compare the oxidant demands and the reactivity of free chlorine and monochloramine toward AAP and 1,4-benzoquinone. Chlorine demands of AAP and 1,4-benzoquinone were much more important than monochloramine demands and respectively accounted for 13.4 (±0.2) and 6.8 (±0.5) mol/mol. The reaction of AAP with monochloramine was monitored using reversed-phase high performance liquid chromatography with ultraviolet absorbance (HPLC-UV). AAP reacted with monochloramine to form simultaneously two first byproducts. The half-life of reaction was estimated to be 90 min. The apparent second-order rate constant (kapp2) for the reaction of AAP with monochloramine at pH 8.5 was 231 M−1·h−1.

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