Simultaneous liquid-chromatographic quantitation of salicylic acid, salicyluric acid, and gentisic acid in plasma.

1979 ◽  
Vol 25 (8) ◽  
pp. 1420-1425 ◽  
Author(s):  
B E Cham ◽  
D Johns ◽  
F Bochner ◽  
D M Imhoff ◽  
M Rowland
Keyword(s):  
Salicylic Acid ◽  
Gentisic Acid ◽  
Salicyluric Acid ◽  
Liquid Chromatographic

Simultaneous liquid-chromatographic quantitation of salicylic acid, salicyluric acid, and gentisic acid in urine.

1980 ◽  
Vol 26 (1) ◽  
pp. 111-114
Author(s):  
B E Cham ◽  
F Bochner ◽  
D M Imhoff ◽  
D Johns ◽  
M Rowland
Keyword(s):  
Salicylic Acid ◽  
Internal Standard ◽  
Peak Height ◽  
Reversed Phase ◽  
Gentisic Acid ◽  
Salicyluric Acid ◽  
Analytical Recovery ◽  
Volume Response ◽  
Assay Precision ◽  
Liquid Chromatographic

Abstract We have developed a specific and sensitive method for the determination of salicylic acid, salicyluric acid, and gentisic acid in urine. Any proteins present are precipitated with methyl cyanide. After centrifugation, an aliquot of the supernate is directly injected into an octadecyl silane reversed-phase chromatographic column, then eluted with a mixture of water, butanol, acetic acid, and sodium sulfate, and quantitated at 313 nm by ultraviolet detection according to peak-height ratios (with internal standard, o-methoxybenzoic acid) or peak heights (no internal standard). The method allows estimates within 25 min. Sensitivity was 0.2 mg/L for gentisic acid, and 0.5 mg/L for both salicyluric and salicylic acid (20-micro L injection volume); response was linear with concentration to at least 2.000 g/L for salicylic acid and metabolites. Analytical recovery of salicylic acid and metabolites from urine is complete. Intra-assay precision (coefficient of variation) is 5.52% at 7.5 mg/L for salicylic acid, 5.01% at 9.33 mg/L for salicyluric acid, and 3.07% at 7.96 mg/L for gentisic acid. Interassay precision is 7.32% at 7.51 mg/L for salicylic acid, 5.52% at 8.58 mg/L for salicyluric acid, and 3.97% at 8.32 mg/L for gentisic acid. We saw no significant interference in urine from patients being treated with various drugs other than aspirin.

Simultaneous liquid-chromatographic quantitation of salicylic acid, salicyluric acid, and gentisic acid in urine.

1980 ◽  
Vol 26 (1) ◽  
pp. 111-114 ◽  
Author(s):  
B E Cham ◽  
F Bochner ◽  
D M Imhoff ◽  
D Johns ◽  
M Rowland
Keyword(s):  
Salicylic Acid ◽  
Internal Standard ◽  
Peak Height ◽  
Reversed Phase ◽  
Gentisic Acid ◽  
Salicyluric Acid ◽  
Analytical Recovery ◽  
Volume Response ◽  
Assay Precision ◽  
Liquid Chromatographic

Abstract We have developed a specific and sensitive method for the determination of salicylic acid, salicyluric acid, and gentisic acid in urine. Any proteins present are precipitated with methyl cyanide. After centrifugation, an aliquot of the supernate is directly injected into an octadecyl silane reversed-phase chromatographic column, then eluted with a mixture of water, butanol, acetic acid, and sodium sulfate, and quantitated at 313 nm by ultraviolet detection according to peak-height ratios (with internal standard, o-methoxybenzoic acid) or peak heights (no internal standard). The method allows estimates within 25 min. Sensitivity was 0.2 mg/L for gentisic acid, and 0.5 mg/L for both salicyluric and salicylic acid (20-micro L injection volume); response was linear with concentration to at least 2.000 g/L for salicylic acid and metabolites. Analytical recovery of salicylic acid and metabolites from urine is complete. Intra-assay precision (coefficient of variation) is 5.52% at 7.5 mg/L for salicylic acid, 5.01% at 9.33 mg/L for salicyluric acid, and 3.07% at 7.96 mg/L for gentisic acid. Interassay precision is 7.32% at 7.51 mg/L for salicylic acid, 5.52% at 8.58 mg/L for salicyluric acid, and 3.97% at 8.32 mg/L for gentisic acid. We saw no significant interference in urine from patients being treated with various drugs other than aspirin.

Improved liquid-chromatography of aspirin, salicylate, and salicyluric acid in plasma, with a modification for determining aspirin metabolites in urine.

1982 ◽  
Vol 28 (5) ◽  
pp. 1200-1203 ◽  
Author(s):  
J N Buskin ◽  
R A Upton ◽  
R L Williams
Keyword(s):  
Salicylic Acid ◽  
Liquid Chromatography ◽  
Plasma Concentration ◽  
Peak Plasma ◽  
Peak Plasma Concentration ◽  
Indirect Measurement ◽  
Gentisic Acid ◽  
Salicyluric Acid ◽  
Performance Specifications ◽  
Liquid Chromatographic

Abstract Detailed performance specifications are given for a specific and sensitive liquid-chromatographic assay for aspirin, salicylic acid, and salicyluric acid in plasma. The sensitivity of this method for aspirin (50 micrograms/L) is 10-fold that of previous methods, so that concentrations of aspirin in plasma can now be followed for about four or five half-lives after the peak plasma concentration arising from a single 650-mg dose. In addition, this assay is as sensitive for salicylic and salicyluric acid in plasma as any hitherto. A modification permits measurement of gentisic acid, salicylic acid, and salicyluric acid in urine; further modifications allow indirect measurement of conjugated gentisate and salicylate in urine.

Metabolism of Aspirin after Therapeutic and Toxic Doses

1990 ◽  
Vol 9 (3) ◽  
pp. 131-136 ◽  
Author(s):  
D.K. Patel ◽  
A. Hesse ◽  
A. Ogunbona ◽  
L.J. Notarianni ◽  
P.N. Bennett
Keyword(s):  
Salicylic Acid ◽  
Therapeutic Dose ◽  
Urinary Metabolites ◽  
Urinary Recovery ◽  
Main Metabolite ◽  
Gentisic Acid ◽  
Salicyluric Acid ◽  
Glycine Conjugate ◽  
Kinetics Of

1 The urinary recovery of metabolites of aspirin (ASA) was studied in 45 volunteers who took a therapeutic dose (600 mg) of ASA by mouth and in 37 patients who took ASA in overdose. 2 The main metabolite recovered from the volunteers was the glycine conjugate, salicyluric acid (SUA), which accounted for 75.01 ± 1.19% of total urinary metabolites, whereas salicylic acid (SA) accounted for 8.82 ± 0.56%. Recovery of SUA was negatively correlated with that of SA (r = -0.8625, P < 0.001). 3 In 24 patients with admission plasma salicylate concentrations of 240-360 mg 1-1, SUA accounted for 46.66 ± 3.22% and SA for 31.88 ± 4.02%. 4 In 13 patients with admission plasma salicylate concentrations of 715-870 mg 1-1, SUA accounted for 21.57 ± 3.65% and SA for 64.72 ± 4.82%. 5 Reduced excretion of salicylate as SUA was also accompanied by increased elimination as gentisic acid and salicylic acid phenolic glucuronide indicating that the unsaturated processes that lead to the formation of these metabolites contribute significantly (22-23%) to the inactivation of large doses of salicylate. 6 While the Michalis-Menten kinetics of ASA have been well demonstrated at lower doses, our findings illustrate the progressive saturation of SUA formation under conditions of increasing ASA load to toxic amounts and raise issues about the in-vivo glycine pool when ASA is taken in overdose.

Liquid Chromatographic Assay for Salicylic Acid in Liquid and Semisolid Formulations

1985 ◽  
Vol 8 (11) ◽  
pp. 2093-2103 ◽  
Author(s):  
A. M. Molokhia ◽  
H. I. Al-shora ◽  
S. Al-rahman
Keyword(s):  
Salicylic Acid ◽  
Liquid Chromatographic

scholarly journals Application of Liquid Chromatography to the Simultaneous Determination of Acetylsalicylic Acid, Caffeine, Codeine, Paracetamol, Pyridoxine, and Thiamine in Pharmaceutical Preparations

2001 ◽  
Vol 84 (3) ◽  
pp. 676-683 ◽  
Author(s):  
Natividad Ramos-Martos ◽  
Francisco Aguirre-Gómez ◽  
Antonio Molina-Díaz ◽  
Luis F Capitán-Vallvey
Keyword(s):  
Salicylic Acid ◽  
Acetylsalicylic Acid ◽  
Simultaneous Determination ◽  
Pharmaceutical Preparations ◽  
Reversed Phase ◽  
Liquid Chromatographic Method ◽  
Relative Standard ◽  
Phase Liquid ◽  
Liquid Chromatographic

Abstract This paper describes a rapid reversed-phase liquid chromatographic method, with UV detection, for the simultaneous determination of acetylsalicylic acid, caffeine, codeine, paracetamol, pyridoxine, and thiamine in pharmaceutical preparations. A reversed-phase C18 Nucleosil column is used. The mobile phase consists of 2 successive eluants: water (5 min) and acetonitrile–water (75 + 25, v/v; 9 min), both adjusted to pH 2.1 with phosphoric acid. Before determination acetylsalicylic acid is completely converted to salicylic acid by alkaline hydrolysis. Salicylic acid, caffeine, paracetamol, pyridoxine, and thiamine are all detected at 285 nm, whereas codeine is detected at 240 nm. Calibration curves were linear for salicylic acid, caffeine, paracetamol, and pyridoxine in the range of 50–500 mg/L, and for codeine and thiamine in the range of 50–1000 mg/L. The method was applied to the analysis of 13 fortified commercial pharmaceutical preparations. Recoveries ranged from 92.6 to 105.5%, with relative standard deviations of 1.1–5.8%.

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