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Abstract

In this thesis we have approached the new chromatographic

techniques like HPLC/UPLC which can improve the analysis throughput

and cycle times. The proficient research work has been divided in to five

chapters. The thesis is composed of four articles, two active

pharmaceutical ingredients, one combination drug product and one

key starting raw material which was selected for the research work.

Keeping in view, the objective to develop new analytical methods for

the determination of related components, assay and enantiomeric

purity.

Chapter-l: Introduction and importance of analytical method

development in pharmaceutical research and development

In this chapter a brief outline on importance of development of novel

liquid chromatographic methods for related components estimation in

pharmaceutical research and development, importance of impurity

evaluation and ICH methodology for stability indicating method

development were explained.

Chapter-2: A validated new chiral LC method for the enantiomeric

separation of vildagliptin

Vildagliptin is a new oral anti-diabetic drug of the dipeptidyl

peptidase-4 inhibitor class of drugs used as a single enantiomer (S).

Galvus is a brand name for Vildagliptin.

This chapter comprised chiral analytical method development and

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method validation of S-vildagliptin and its other enantiomer by HPLC.

Chapter-3: Simultaneous determination of Sitagliptin phosphate

monohydrate and Metformin hydrochloride in tablets by validated

ultra performance liquid Chromatography Method

Sitagliptin phosphate monohydrate and Metformin hydrochloride are

oral anti-diabetic drugs. Sitagliptin phosphate is used for the

improvement of glycemic control in patients with type II diabetes mellitus

as monotherapy or combination therapy with metformin when the single

agent does not provide adequate glycemic control. The brand name is

Janumet.

This chapter comprised analytical method development for the

simultaneous determination of sitagliptin phosphate monohydrate and

metformin hydrochloride in pharmaceutical dosage forms and its

analytical method validation by HPLC.

Chapter-4: A validated LC method for the determination of chiral

purity of (S)-2-azido-3-methylbutanoic acid: a key raw material of

Valganciclovir hydrochloride

(S)-2-azido-3-methylbutanoic acid is a single enantiomer and very

critical as it affects the overall chiral purity of Valganciclovir

hydrochloride. Valganciclovir hydrochloride is an antiviral drug. The

brand name is Valcyte.

This chapter comprised chiral analytical method development and

method validation of (S)-2-azido-3-methylbutanoic acid and its other

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enantiomer by HPLC.

Chapter-5: A stability indicating UPLC method for the rapid

separation of related components of Gemcitabine hydrochloride

Gemcitabine hydrochloride is a chemotherapeutic agent that works by

slowing or stopping the growth of cancer cells and marketed as Gemzar

by Eli Lilly and company.

This chapter comprised analytical method development for process

related impurities, degradation products in Gemcitabine API and its

analytical method validation by HPLC.