Determination of Salicylic Acid and Two Metabolites in Plasma and Urine Using Fluorimetry for Directly Measuring Salicyluric Acid

Author(s):  
Edward B. Truitt ◽  
Ann M. Morgan ◽  
J. Maxwell Little
1975 ◽  
Vol 21 (8) ◽  
pp. 1167-1168 ◽  
Author(s):  
Nagy A Farid ◽  
Gordon S Born ◽  
Wayne V Kessler ◽  
S M Shaw ◽  
W E Lange

Abstract We describe an improvement in the Levy and Procknal method [J. Pharm. Sci. 57, 1330 (1968)] for determination of salicylic acid and its metabolites in urine. Salicylic acid and salicyluric acid are successively extracted from 1 or 2 ml of urine (acidified with HCl) by two 10-ml portions each of carbon tetrachloride and ethylene dichloride. The extracts of each solvent are shaken with 5 ml of ferric nitrate solution (a 10-fold dilution of 17 g of Fe(NO3)3·9H2O in 1 liter of 70 mmol/liter HNO3). The aqueous phases are centrifuged and their absorbances measured at 530 nm. For total salicylate, 3 ml of urine and 3 ml of HCl are heated in a partially evacuated serum vial at 100 °C for 16 h and then salicylic acid is assayed in the hydrolyzed sample. Recovery of a weighed oral dose of sodium salicylate in urine was 105.4%; it was 127.9% by the Levy and Procknal method for the same sample. The improved method is faster and more accurate.


1977 ◽  
Vol 10 (7-8) ◽  
pp. 539-550 ◽  
Author(s):  
Ihor Bekersky ◽  
Harold G. Boxenbaum ◽  
Marian H. Whitson ◽  
Carl V. Puglisi ◽  
Robert Pocelinko ◽  
...  

Soil Research ◽  
1989 ◽  
Vol 27 (4) ◽  
pp. 663 ◽  
Author(s):  
EA Close ◽  
HKJ Powell

This paper examines the use of short extraction times, and the determination of aluminium with chrome azurol S (CAS), for the estimation of 0.02 M CaCl2-soluble aluminium in soils. It reports the correlation between CAS-reactive aluminium in 5 min extracts and percent maximum yield of white clover (Trifolium repens) for a series of acid soils. The reactivity of soluble and colloidal aluminium species with the metallochromic reagent CAS has been assessed. ~ l ( a q ) ~ + , simple hydroxy species and complexes of weakly binding ligands (salicylic acid, tannins) are CAS-reactive (2 rnin). In contrast, complexes of strongly binding ligands (citric acid, fulvic acid) are not CAS-reactive ([Al] ~ [L] ~ [CAS] ~ 1-2~10-5 M). For a series of six limed phosphated topsoils and subsoils (pH 4.2-5.5), 0.02 M CaCl2- soluble aluminium, as determined with CAS, was negatively correlated against the percent maximum yield of white clover; r2 = -0.73** (5 min extraction), n = 20. This correlation is similar to that for yield against total aluminium as determined by atomic absorption spectroscopy after 60 min extraction (r2 = -0.77**). However, the colorimetric analysis is more convenient and sensitive; further, it does not measure colloidal and polymeric aluminium species (which may not be plant-available). The satisfactory correlation achieved for short extraction times suggests use of CAS for a rapid field method for aluminium toxicity in soils.


2001 ◽  
Vol 84 (3) ◽  
pp. 676-683 ◽  
Author(s):  
Natividad Ramos-Martos ◽  
Francisco Aguirre-Gómez ◽  
Antonio Molina-Díaz ◽  
Luis F Capitán-Vallvey

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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