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Abstract

Simultaneous estimation of parent and its metabolite(s) in a single method poses a threat when one has to monitor one mass transition while running the other compound on liquid chromatographymass spectrometer. This would again become critical once interference is observed at the retention time of compound of interest in-spite of its absence in the sample. In this paper, a selective and sensitive liquid chromatography-tandem mass spectrometry method for the simultaneous determination of Raloxifene and its two active metabolites, Raloxifene 4-Glucuronide and Raloxifene 6-Glucuronide in human plasma was developed and validated. The method involves a rapid solid-phase extraction from plasma, followed by reversed-phase chromatography with gradient flow condition and mass spectrometry detection. Validation parameters were selected ranging from 0.016 to 1.187 ng/mL for Raloxifene, 3.073 to 700.558 ng/mL Raloxifene 4-Glucuronide and 0.311 to 124.526 ng/ml for Raloxifene 6-Glucuronide. The mean recovery for Raloxifene, Raloxifene 4-Glucuronide, and Raloxifene 6-Glucuronide found to be 85.10, 86.30 & 87.20%, respectively. The peak concentration of Raloxifene, Raloxifene 4-Glucuronide, and Raloxifene 6-Glucuronide were 0.330 ng/mL, 153.047 ng/mL and 27.744 ng/mL respectively for the reference product, in fasted conditions. INTRODUCTION: Raloxifene is a selective estrogen receptor modulator (SERM) having selective agonist or antagonist activities on tissues responsive to estrogen. In postmenopausal women with osteoporosis, Raloxifene reduces the incidence of vertebral fractures, preserves bone mass, and increases bone mineral density (BMD) 1-3 .

Development and Validation of Total Levothyroxine and Total Liothyronine in Human Serum using Chemiluminescence Micro Particle Immunoassay and Its Application to Bioequivalence Study

“…ISR is the way to assess any bioanalytical method reproducibility for the unknown samples and numerous of regulatory recommendations and various publications suggest repeat of random study samples as the incurred samples [18][19][20][21][22][23][24][25][26] . A validated method, which is reproducible demonstration and proper evaluation of incurred sample reproducibility and stability is essential to produce a reliable study data.…”