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Chapter 6

This document discusses conclusions from analytical chemistry methods developed for several pharmaceutical drugs. Rapid and sensitive methods were successfully developed using HPLC to simultaneously quantify drugs like lamivudine, tenofovir, and dolutegravir, as well as sofosbuvir and velpatasvir. A stability-indicating method was also developed for fosamprenavir calcium. All the developed methods were validated, economical, accurate, and suitable for routine quality control analysis of pharmaceutical products.

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40 views4 pages

Chapter 6

This document discusses conclusions from analytical chemistry methods developed for several pharmaceutical drugs. Rapid and sensitive methods were successfully developed using HPLC to simultaneously quantify drugs like lamivudine, tenofovir, and dolutegravir, as well as sofosbuvir and velpatasvir. A stability-indicating method was also developed for fosamprenavir calcium. All the developed methods were validated, economical, accurate, and suitable for routine quality control analysis of pharmaceutical products.

Uploaded by

S.K. MISHRA
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Download as PDF, TXT or read online on Scribd
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Overall Conclusions

Chapter 6

Overall Conclusions

108
Overall Conclusions

Pharmaceutical Analytical Chemistry is an important part in monitoring the


quality of pharmaceutical products for safety and efficacy. The current trends in
Pharmacopeias rely more on instrumental techniques rather than the classical wet
chemistry methods. This has resulted in the availability of indigenous instruments like
spectrophotometer, high performance liquid chromatography (HPLC), gas
chromatography (GC) and Ultra performance liquid chromatography (UPLC) etc in
almost all analytical laboratories and pharmaceutical companies. Due to the advent of
automation, small sample size and high sensitivity of the instrument, very accurate and
precise assay and degradation products methods can be developed on chromatographic
instruments with a considerable reduction in the total analysis time. With these
advancements in analytical techniques, the ability to develop methods with short run time
and relatively simple sample procedure for simultaneous estimation of individual drugs
and as well as in combination drug product is central to the role of analytical chemists.

In the present work, a stability indicating RP-HPLC method was successfully


developed and validated for the determination of single or combined dosage form and
estimation of degradants generated during the formulation. The pharmaceutical drugs
such as, Lamivudine, Tenofovir DF and Dolutegravir; Sofosbuvir and Velpatasvir;
Fosamprenavir calcium; and Calcium dobesilate were effectively estimated and the
obtained results and discussions are presented in Chapter 2, Chapter 3, Chapter 4 and
Chapter 5, respectively.

A rapid, sensitive and accurate method was to develop and validate for
simultaneous estimation of Lamivudine, Tenofovir DF and Dolutegravir in drug
product by liquid chromatography. The chromatographic separation was achieved on
column (Luna C8 150*4.6 mm) at ambient temperature .The separation was achieved
employing a mobile phase consists of 0.1%v/v TFA in water and Acetonitrile with simple
gradient programme. The flow rate was maintained as 1.0 mL/min and ultra violet
detector at 260 nm was used. The average retention time for Lamivudine, Tenofovir DF
and Dolutegravir found to be 2.023 min, 5.330 min and 7.673. The proposed method
was validated for selectivity, precision, linearity and accuracy. All validation parameters

109
Overall Conclusions

were within the acceptable range. The assay methods were found to be linear from 75.0 –
225.0 μg/mL for Lamivudine, 75.0 – 225.0 μg/mL of Tenofovir DF and 12.5 – 37.50
μg/mL of Dolutegravir. From the results, the proposed method is more acceptable and
cost effective and it can be effectively applied for routine analysis in research institutions,
quality control department in industries and approved testing laboratories.

The pharmaceutical drugs, Sofosbuvir and Velpatasvir were determined by a


rapid and sensitive reverse phase high performance liquid chromatography method. The
method is found to be simple, precise, economical, accurate, reproducible, and sensitive.
The chromatographic separation was achieved on the C18 column (Luna 18 150*4.6
mm3.0 um) at ambient temperature. The separation achieved employing a mobile phase
consists of 0.1%v/v formic acid in water: methanol:acetonitrile (35:40:25). The flow rate
was 0.8 mL/min and ultraviolet detector at 269 nm was used. The average retention time
for velpatasvir and sofosbuvir found to be 2.62 min and 3.72 min. Further, the developed
method was validated as per the ICH analytical method validation guidelines. All
validation parameters were within the acceptable range. The assay methods were found to
be linear from 80 to 240 μg/mL for Sofosbuvir and 20–60 μg/mL for Velpatasvir. The
correlation coefficient was 0.9998 and 0.9992 for Velpatasvir and Sofosbuvir
respectively. The mean percentage recovery for the developed method was found to be in
the range of 98.4–100.4% for Velpatasvir and 98.6–100.6% for Sofosbuvir. The
developed method was found to be suitable for the routine quantitative analysis of
Velpatasvir and Sofosbuvir in bulk and pharmaceutical dosage form. It was also
concluded that developed method was accurate, precise, linear, reproducible, robust, and
sensitive.

A reversed phase HPLC method is proposed for the estimation of Fosamprenavir


in the presence of its impurities and degradation products. The drug substance was
subjected to stress conditions of hydrolysis, oxidation, photolysis and thermal
degradation. The drug was found to be stable in other stress conditions studied.
Successful separation of the drug from the process impurities and degradation products
formed under stress conditions were achieved on an Xbridge Phenyl (250 x 4.6 mm) 5

110
Overall Conclusions

μm column. The gradient LC method employs solution A and solution B as mobile phase.
The solution A contains aqueous 0.1% TFA in Water and solution B contains acetonitrile
as Gradient mode. The HPLC method was developed and validated with respect to
linearity, accuracy, precision, specificity and ruggedness. Further, the simple, precise,
accurate and high resolution and shorter retention time makes this method more
acceptable and cost effective and it can be effectively applied for routine analysis in
research institutions, quality control department in meant in industries, approved testing
laboratories for the determination of Fosamprenavir drug.

A new, simple, rapid, selective, precise and accurate isocratic reverse phase high
performance liquid Chromatography assay method has been developed for estimation of
Calcium dobesilate in tablet formulations. The separation was achieved by using column
Waters symmetry C18 (4.6x150mm), 5μ (Make: Waters), in mobile phase consisted of
pH 2.5 Phosphate buffer Acetonitrile and in the ratio of (95:5, v/v). The flow rate was 1.0
mL.min-1 and column oven temperature 30°C, the injection volume was 20 μL the
separated Calcium dobesilate was detected using UV detector at the wavelength of 300
nm. The retention time of Calcium dobesilate, was noted to be 4.22 min, indicative of
rather shorter analysis time. The method was validated as per ICH guidelines. The
proposed method was applied for determination of Calcium dobesilate in marketed
formulation. Hence, the developed RP-HPLC method was found to be satisfactory and
could be used for the routine analysis of Calcium dobesilate in tablet dosage form.

111

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