A validated HPLC method with electrochemical detection for simultaneous assay of 5‐aminosalicylic acid and its metabolite in human plasma

Abstract

A high-performance liquid chromatographic method was developed, validated and applied to the simultaneous determination of 5-aminosalicylic acid (5-ASA) and its acetylated metabolite (acetyl-5-ASA) in human plasma. The method involves liquid-liquid extraction with methanol followed by isocratic reversed-phase chromatography on a Kromasil KR100 C(18) column with electrochemical detection. The recovery, selectivity, linearity, precision and accuracy of the method were evaluated from spiked human plasma samples. The effects of mobile phase composition, buffer concentration, mobile phase pH and concentration of organic modifiers on retention of 5-ASA, acetyl 5-ASA and internal standard were investigated. Limits' of detection were 5 ng/mL for 5-ASA and 10 ng/mL for acetyl-5-ASA, respectively. The method can be used for supporting therapeutical drug monitoring and pharmacokinetic studies.

Development and validation of a HPLC-ESI-MS/MS method for the determination of 5-aminosalicylic acid and its major metabolite N-acetyl-5-aminosalicylic acid in human plasma

“…A number of analytical methods have been developed for the analysis of 5-ASA and its metabolite in many biological matrices, e.g. plasma [16,[18][19][20][21][22][23], serum [24], feces [24], urine [18,19,[22][23][24], stones [25] and rectal biopsies [23,24]. These methods include HPLC combined with UV [16,[25][26][27], fluorescence (FL) [14][15][16]18,20,28,29], and electrochemical (EC) [21] detections.…”

Determination of mesalamine by spectrofluorometry in human serum after solid-phase extraction with Ni-Al layered double hydroxide as a nanosorbent

“…1 A number of analytical methods has been developed for the analysis of mesalamine in pharmaceutical dosage forms and biological matrices. These methods include voltammetry, 2-4 spectrophotometry, 5,6 spectrofluorometry, 7,8 coulometery, 9 and high-performance liquid chromatography (HPLC) combined with UV, [10][11][12] fluorescence, 13,14 mass spectrometry (MS), 15, 16 and electrochemical (EC) 17 detections. Mesalamine is usually present at trace levels in a complex biological matrix, and the potentially interfering endogenous substances (which are usually present at higher concentrations than the drug) need to be removed before the analysis.…”

Simple and sensitive spectrophotometric methods for the analysis of mesalamine in bulk and tablet dosage forms

“…8 Various other techniques such as UVspectrophotometry, 9 potentiometric titration, 10 micellar electrokinetic chromatography, 11 differential pulse voltammetry, 12 HPLC and LC/ MS/MS have been reported for assaying of MSL in pharmaceutical dosage forms and biological fluids. [13][14][15][16][17][18][19][20][21][22][23][24][25][26] Visible spectrophotometry, because of simplicity and cost effectiveness, sensitivity and selectivity and fair accuracy and precision, has remained competitive in the era of chromatographic techniques for pharmaceutical analysis. Few visible spectrophotometric methods are found in the literature for the assay of MSL.…”