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  • Simultaneous determination of 5-aminosalicylic acid, acetyl-5-aminosalicylic acid and 2,5-dihydroxybenzoic acid in endoscopic intestinal biopsy samples in humans by high-performance liquid chromatography with electrochemical detection.

Simultaneous determination of 5-aminosalicylic acid, acetyl-5-aminosalicylic acid and 2,5-dihydroxybenzoic acid in endoscopic intestinal biopsy samples in humans by high-performance liquid chromatography with electrochemical detection.

Journal of pharmaceutical and biomedical analysis (1995-12-01)
G Palumbo, G Carlucci, P Mazzeo, G Frieri, M T Pimpo, D Fanini
ABSTRACT

A high-performance liquid chromatographic method for the simultaneous determination of 5-aminosalicylic acid (5-ASA), acetyl-5-aminosalicylic acid (Ac-5-ASA) and 2,5-dihydroxybenzoic acid (5-HSA) in human endoscopic intestinal biopsy with electrochemical detection has been developed and validated. A liquid-liquid extraction procedure was used to isolate these drugs from the biological material prior to analysis. The compounds were separated on an Erbasil S reversed-phase column using methanol-critic acid-sodium hydrogenphosphate-heptane-sulfonic acid-disodium ethylenediaminetetraacetate (pH 3) as mobile phase. The method was linear from 1.0 to 300 ng ml-1 for 5-ASA, from 10 to 1000 ng ml-1 for Ac-5ASA and from 0.1 to 10 ng m-1 for 5-HSA. The limit of detection for 5-ASA and for Ac-5-ASA was 1 ng ml-1 and that for 5-HSA was 0.1 ng ml-1. This procedure is suitable for pharmacological and clinical studies of 5-ASA.

MATERIALS
Product Number
Brand
Product Description

Supelco
2,5-Dihydroxybenzoic acid, analytical standard
Sigma-Aldrich
2,5-Dihydroxybenzoic acid, 98%
Supelco
2,5-Dihydroxybenzoic acid, matrix substance for MALDI-MS, >99.0% (HPLC)
Supelco
2,5-Dihydroxybenzoic acid, matrix substance for MALDI-MS, ≥99.5% (HPLC), Ultra pure