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Title: Development of enantioselective assay and evaluation of pharmacokinetic properties of lenalidomide by HPLC & LC-MS/MS
Researcher: Krishna Pocha
Guide(s): Devala Rao, G
Keywords: Bio Technology
Upload Date: 23-Apr-2013
University: Acharya Nagarjuna University
Completed Date: 2011
Abstract: Immobilised polysaccharide based chiral stationary phase (CSPs) are a new generation of chromatographic materials combining the remarkable enantioselective performance of the polysaccharide derivatives and solvent versatility for enantiomeric resolution. Based on extensive experimental work, this work will focus on the approach to efficient method development with these Immobilised CSPs (Chiralpak IA, Chiralpak IB and Chiralpak IC) by applying a limited number of mobile phases. The experiments were performed under normal phase conditions. The influence of polar modifier, mobile phase composition, flow rate and column temperature on the etention time and separation factor behavior of Thalidomide (TLM) and Lenalidomide (LLM) was evaluated. Apparent thermodynamic parameters were also deduced from Van t Hoff plots, and some aspects of chiral recognition mechanism were studied. Lenalidomide, 3-(4-amino-1-oxo-3H-isoindol-2-yl) piperidine-2,6-dione, currently on the market and in therapeutic use as a racmate. In order to investigate single enantiomers of lenalidomide in pharmaceutical formulations both were chromatographically purified and characterized. High Performance Liquid Chromatography (HPLC) has enantiomerically separated the two enantiomers of lenalidomide (LLM) at semi-preparative scale on a polysaccharide based chiral stationary phase (Chiralpak IC, 250x10 mm, and 5 µm). The effect of organic modifier (2-propanol) was studied, and different injection volumes and concentrations of the lenalidomide racemic mixture were evaluated in order to obtain high enantiomeric purities. Better results were achieved using concentration overloading instead of volume overloading. The recoveries decreased when the requirements of enantiomeric purity or the load increased, but it was possible to recover gt99.1% of both enantiomers at an enantiomeric purity higher than gt99.60% under some loading conditions, like injecting 1 ml of a solution of 6 g/lit.
Pagination: 183p.
Appears in Departments:Department of Bio Technology

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01_title.pdfAttached File148.53 kBAdobe PDFView/Open
02_certificate.pdf13.75 kBAdobe PDFView/Open
03_declaration.pdf12.51 kBAdobe PDFView/Open
04_acknowledgement.pdf15.46 kBAdobe PDFView/Open
05_dedication.pdf12.49 kBAdobe PDFView/Open
06_list of symbols and abbreviations.pdf21.43 kBAdobe PDFView/Open
07_list of tables.pdf28.11 kBAdobe PDFView/Open
08_list of figures.pdf46.77 kBAdobe PDFView/Open
09_contents.pdf11.38 kBAdobe PDFView/Open
10_abstract.pdf38.36 kBAdobe PDFView/Open
11_literature review.pdf46.23 kBAdobe PDFView/Open
12_objective.pdf28.88 kBAdobe PDFView/Open
13_approach.pdf16.01 kBAdobe PDFView/Open
14_chapter 1.pdf554.3 kBAdobe PDFView/Open
15_chapter 2.pdf672.94 kBAdobe PDFView/Open
16_chapter 3.pdf461.12 kBAdobe PDFView/Open
17_chapter 4.pdf1.06 MBAdobe PDFView/Open
18_chapter 5.pdf170.54 kBAdobe PDFView/Open
19_chapter 6.pdf629.14 kBAdobe PDFView/Open
20_chapter 7.pdf336.11 kBAdobe PDFView/Open
21_conclusion.pdf40.04 kBAdobe PDFView/Open

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