WJPR Citation New

  All Since 2011
 Citation  2903  2393
 h-index  27  24
 i10-index  68  60

Login

Best Paper Awards

World Journal of Pharmaceutical Research (WJPR) will give best paper award in every issue in the form of money along with certificate to promote research activity of scholar.
            Best Paper Award :
Dr. Muhammad Baqir MR Fakhrildin
Download Article: Click Here

Search

Track Your Article

Abstract

AN IMPROVED STABLE ISOTOPE LIQUID CHROMATOGRAPHY TANDEM MASS SPECTROMETRY METHOD FOR THE DETERMINATION OF N-ACETYL-5-AMINOSALICYLIC ACID AND ITS DERIVATIZED PARENT, 5-AMINOSALICYLIC ACID IN HUMAN PLASMA

Mubarak Hasan Shah*, Padmanabha Reddy Yeragam Reddy and
Madhira Bhawanishankar

ABSTRACT

A new stable isotope LC-MS/MS for the determination of 5- aminosalicylic acid (5-ASA) and N-acetyl-5-ASA in human plasma was developed and validated. The objective of this study was to develop and validate an improved selective LC-MS/MS method for the simultaneous determination method of 5-ASA as its derivatized product, N-propionyl-5-ASA along with its principal phase II acetylated metabolite, N-acetyl-5-ASA using 5-ASA D3 and N-acetyl- 5-ASA D3 as internal standards. Derivatization step is necessary to convert the ionizable amino group to non ionizable N-propionyl amino moiety in 5-ASA and 5-ASA D3 by using propionic anhydride, followed by liquid-liquid extraction with ethyl acetate (acidified medium) from human plasma. Lower limit of quantification was found to be 5 ng/mL and 7.5 ng/mL for 5-ASA and N-acetyl-5-ASA respectively. The temperature of column and autosampler were maintained at 40°C and 4°C, respectively. The method validation were carried out as per the USFDA guidelines as described, showing a linearity system (r 2 > 0.99) over a range of 5 ng/mL to 1000 ng/mL for 5-ASAand 7.5 ng/mL to 1500 ng/mL concentrations for N-acetyl-5-ASAand a recovery shows 98.8% and 78.8% for 5-ASA and N-acetyl-5-ASA respectively. Intra-assay and inter-assay precision and accuracy data were within the acceptable range. Stability studies indicate that both 5-ASA and N-acetyl-5- ASA were reasonably stable within the given test condition. The deuterated internal standards used in the study helped in overall assay performance and the accuracy of the data This validated method can be successfully applied for the quantification of 5-ASA and its acetylated metabolite to support pharmacokinetic or bio-studies.

Keywords: 5-ASA, N-acetyl-5-ASA, LC-MS/MS Method validation.


[Full Text Article]

Call for Paper

World Journal of Pharmaceutical Research (WJPR)
Read More

Email & SMS Alert

World Journal of Pharmaceutical Research (WJPR)
Read More

Article Statistics

World Journal of Pharmaceutical Research (WJPR)
Read More

Online Submission

World Journal of Pharmaceutical Research (WJPR)
Read More