Estimation of Mesalamine in Human Plasma Using Rapid and Sensitive LC-ESI-MS/MS Method

Abstract

A sensitive, selective and rapid liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS) method has been developed for the estimation of mesalamine in human plasma using a derivatization technique. A liquid-liquid extraction technique with ethyl acetate was used for the extraction of mesalamine and mesalamine-D3 internal standard (IS). Mesalamine and mesalamine-D3 were analyzed on Thermo BetaBasic C8 (100 mm ´4.6 mm, 5 mm) column using acetonitrile and 10 mM ammonium formate in 70 : 30 v/v ratio under isocratic elution mode. The MS detection and quantitation were performed under multiple reaction monitoring using positive ESI for mesalamine (m/z, 210.1 ® 191.9) and mesalamine D3 (m/z, 213.2 ® 195.1). Main advantages of the proposed method include higher sensitivity (5.00 ng/mL), superior extraction efficiency (³79%), and small volume (200 mL) of sample for processing. The calibration curve was linear in the concentration range of 5.00 -2957.17 ng/mL with a good correlation coefficient (r 2 ³ 0.9980) for mesalamine. The intra-batch (within day) and inter-batch (between days) precision (% CV) and accuracy (% nominal) values varied from 2.09 to 4.44% and from 96.02 to 103.23%, respectively. The method was validated as per the US FDA guidelines and the results were found accurate and precise.

Spectrophotometric Determination of Mesalazine Based on Schiff Base ‎Formation with 2,4-dimethoxybenzaldehyde and 3,4-dihydroxybenzaldehyde.

“…The liquid chromatographyelectrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS) method was developed to detect mesalamine in human plasma. (Pathan and Kshirsagar, 2021). An HPLC approach with fluorometric detection was used to find mesalazine in human plasma (Ceylan et al, 2022).…”