Development and Validation of a RP-HPLC Method for Simultaneous Estimation of Duloxetine and Methylcobalamin in Bulk and Tablet Dosage Form | Chapter 6 | Pharmaceutical Science: New Insights and Developments Vol. 7

 

A simple, robust, precise, and accurate stability-indicating reverse-phase high-performance liquid chromatographic (RP-HPLC) method was successfully developed and validated for the simultaneous estimation of Duloxetine (DLU) and Methylcobalamin (MCB) in their combined pharmaceutical dosage form. The chromatographic analysis was performed on an Inertsil C18 column with dimensions 4.6 × 250 mm and particle size 5 µm, utilising an isocratic elution technique. The mobile phase consisted of a phosphate buffer adjusted to pH 4.5, which facilitated adequate separation of the analytes. The flow rate of the mobile phase was maintained at 1.0 mL/min, and detection of the eluted components was carried out at a wavelength of 255.0 nm using a UV detector. Under the optimised chromatographic conditions, Duloxetine and Methylcobalamin were eluted at retention times of approximately 5.32 minutes and 3.59 minutes, respectively. The developed method showed excellent linearity over the concentration ranges of 20–120 µg/mL for Duloxetine and 10–60 µg/mL for Methylcobalamin. The correlation coefficients (r²) for both analytes were found to be 0.999, indicating a strong linear relationship between peak area and concentration within the specified ranges. Method accuracy was assessed by recovery studies, which demonstrated mean percentage recoveries of 99.68% for Duloxetine and 100.3% for Methylcobalamin, confirming the accuracy of the method. The relative standard deviation (RSD) values for both analytes in recovery studies were found to be not more than 2% (NMT 2%), reflecting high precision and reproducibility of the method. Precision was further evaluated by conducting intra-day and inter-day studies, both of which showed RSD values within acceptable limits (NMT 2%) for both drugs, supporting the reliability and repeatability of the method over different days and time intervals.

 

The developed RP-HPLC method was validated as per the International Council for Harmonisation (ICH) guidelines, ensuring that all critical parameters, including specificity, linearity, accuracy, precision, robustness, and system suitability, were thoroughly assessed and met the established acceptance criteria. The proposed method is therefore considered suitable for the routine quality control and stability analysis of Duloxetine and Methylcobalamin in their combined dosage forms.

 

Author(s) Details

Kandiboti Lavanya
Department of Pharmaceutical Analysis, Sir C. R. Reddy College of Pharmaceutical Sciences, Eluru, Andhra Pradesh, India.

 

V. Anitha Kumari
Department of Pharmaceutical Analysis, Sir C. R. Reddy College of Pharmaceutical Sciences, Eluru, Andhra Pradesh, India.

 

V. Srinivasa Rao
Department of Pharmacy Practice, Lydia College of Pharmacy, Ravulapalem, Andhra Pradesh, India.

 

Please see the book here:- https://doi.org/10.9734/bpi/psnid/v7/5962

QbD Approach to Stability Indicating HPLC Method for Estimation of Elbasvir and Grazoprevir by Green Assessment Method | Chapter 4 | Pharmaceutical Science: New Insights and Developments Vol. 2

Introduction: Green chemistry is widely used in worldwide manufacturing, government policy, educational practice, and technology development. The main purpose of the circular economy is to establish a balance between economic growth, resource sustainability, and environmental protection. The global need to adapt procedures to meet the objectives of green analytical chemistry (GAC) is a serious challenge for the pharmaceutical industry. High-performance liquid chromatography (HPLC), one of the techniques used most commonly at various stages in the pharmaceutical industry, generates a massive volume of organic hazardous waste.

Aim: To develop analytical quality by design-aided stability indicating green high-performance liquid chromatography (HPLC) method for estimation of Elbasvir and Grazoprevir in a dosage form.

Materials and Methods: The percentage of ethanol in the mobile phase, flow rate, and their overall impact on the responses, such as asymmetry, theoretical plates, and resolution, were the crucial chromatographic elements that were examined in order to optimise the procedure. The primary goal of green analytical chemistry (GAC) has been to provide environmentally safe analytical techniques. Consequently, the application of GAC principles in pharmacological analysis is essential. A rotatable central composite design was used, and the Zorbax C18 column (4.6 x 150 mm, 5 µm) with 0.1% Trifluoroacetic acid and ethanol (40:60 v/v) as components of a mobile phase flowing at a rate of 1.0 ml/minute was used to create the ideal conditions for chromatographic separation with a run time of 5 minutes. At 253 nm, photodiode array detection was performed.

Results: The retention times for EBS and GZP were 1.8 and 2.84 minutes, respectively. According to ICH recommendations, the proposed approach was validated, and stress tests demonstrated that Elbasvir and Grazoprevir are sensitive to acidic, basic, and oxidative stress conditions. An analytical eco-scale score evaluated the greenness profile, while a software-based evaluation.

Conclusion: The developed HPLC method is eco-friendly and shall be adopted in the routine quality control of Elbasvir and Grazoprevir in a tablet dosage form. The implementation of the green strategies in the pharma analysis will provide benefits for the analysts' healthier working environment, this technique will also help commercial and industrial lab research and testing departments adopt and evaluate the various combinations in bulk and dosage forms.

 

Author (s) Details

 

Charushila Bhangale
Department of Pharmaceutical Chemistry, Pravara Rural Education Society, College of Pharmacy for Women, Chincholi, Nashik, Maharashtra, India.

 

Sachin Somwanshi
Department of Pharmaceutical Chemistry, Pravara Rural Education Society, College of Pharmacy for Women, Chincholi, Nashik, Maharashtra, India.

 

Kiran Kotade
Department of Pharmaceutical Chemistry, Pravara Rural Education Society, College of Pharmacy for Women, Chincholi, Nashik, Maharashtra, India.

 

Mayur Gaikar
Department of Pharmaceutical Chemistry, Pravara Rural Education Society, College of Pharmacy for Women, Chincholi, Nashik, Maharashtra, India.

 

Please see the book here:-https://doi.org/10.9734/bpi/psnid/v2/4074  

 

Developing a Stability Indicating Ultra Performance Liquid Chromatographic Method for Simultaneous Quantitation of Degradation Products of Telmisartan and Hydrochlorothiazide in Combination Dosage Form | Chapter 3 | Advanced Concepts in Pharmaceutical Research Vol. 9

 

Telmisartan (TLM) is an angiotensin receptor blocker (ARB) that has an extensive period of working and has the lengthy half-life of any ARB. Telmisartan works by blocking a substance in the body that causes blood vessels to tighten. This work is intended to thrive a stability-indicating Ultra performance liquid chromatographic method for the estimation of Telmisatam (TLM) and Hydrochlorothiazide (HCTZ) and degradation products pharmaceutical dosage forms. Separation was carried out on Zorbax Eclipse XDB C-18(50 x mm, 1.7 µm) column using a gradient method. Mobile phase A is 10mM KH2PO4 having 1% (v/v) of trimethylamine and mobile phase B is acetonitrile used in this work. 0.5 mL/ minute is the flow rate and at 271 nm noticed wavelength is monitored. Method development trails were carried out on six different columns. For specificity, limit of quantification, limit of detection, linearity, accuracy, method precision, robustness and stability this method is validated. The correlation coefficient of the impurities is more than 0.99. The stability indicating method confirmed that there was no interference of all impurities of TLM and HCTZ. TLM and HCTZ tablet samples stored and long-term storage conditions. The effect of storage conditions results proved that the method has stability indicating capability. Hence, the developed LC method was stability indicating and well applied for drug product stability study as well as for quality monitoring.

Author(s) Details:

Narasimha Reddy G. P,
Department of Chemistry, Sri Krihnadevaraya University Anantapur, Anantapuramu, Andhra Pradesh, India.

 

Sreenivasulu Reddy T.
Department of Chemistry, Sri Krihnadevaraya University Anantapur, Anantapuramu, Andhra Pradesh, India.


Sidda Reddy K.
Department of Chemistry, Sri Krihnadevaraya University Anantapur, Anantapuramu, Andhra Pradesh, India.

Shashi Kumar K. N.
Department of H&S, Annamacharya Institute of Technology & Sciences, Kadapa, 516003, Andhra Pradesh, India.


Please see the link here: https://stm.bookpi.org/ACPR-V9/article/view/14362

Estimation of Ribociclib and Letrozole in Solid Dosage form (Tablet): A Novel Analytical Method | Chapter 9 | Current Overview on Pharmaceutical Science Vol. 9

An attempt was created to develop a plain, rapid, and corroborated method for the concurrent estimation of ribociclib and letrozole together tablet portion of drug or other consumable form.Inhibitors of cyclin D1/CDK4 (Cyclin-dependent kinase 4) [2] and CDK6 (Cyclin-weak kinase 6) [2] are found in Ribociclib, which is retailed by Novartis under the brand names Kisqali and Kryxana. This drug is used to treat some types of feelings cancer. The mixture of aromatase inhibitors and fulvestrant Inhibitors of cyclin D1/CDK4 (Cyclin-dependent kinase 4) and CDK6 (Cyclin-reliant kinase 6) are found in Ribociclib, This drug is used to treat few types of breast malignancy. The combination of aromatase inhibitors and fulvestrant.The chromatographic break-up was carried out on Waters, proportion C18 (150 mm×4.6 mm with 3.5 µm), travelling phase secondhand was a mixture of safeguard and acetonitrile in the ratio of 80:20, accompanying flow rate of 1ml/min and dose volume of 10 µL for the assay. The detection was finished using PDA at 260 nm, accompanying run time of 5 brief time period. The retention opportunity for the drugs ribociclib and letrozole was detected expected 2.648 min and 3.151 brief time period, respectively. The pattern was validated in accordance with ICH guidelines.The extent of object of letrozole and ribociclib was observed expected in the range of 0.50–7.50 and 40.01–600.15, Correlation coefficient (r2) 0.999 and 0.9983, individually. Accuracy for ribociclib and letrozole is carried out by repeatable concentrations of 50%, 100%, and 150. Validation determinants of robustness and masculinity were detected to be in limits.The grown method was plain, rapid, and logical; it can be secondhand for the simultaneous belief of ribociclib and letrozole tablet portion of drug or other consumable form in routine analysis. The approved method maybe used for the routine reasoning of both the drugs from size and different formulations and will help in healing drug monitoring (TDM) and bioavailability studies.

Author(s) Details:

Bhagyalata Satapathy,
The Tamil Nadu Dr. M.G.R Medical University, India.

Chaitanya Bangari,
The Tamil Nadu Dr. M.G.R Medical University, India.

Please see the link here: https://stm.bookpi.org/COPS-V9/article/view/10178

Developing an Analytical Method and Validation for Estimation of Residual Solvents in Gliclazide Using Gas Chromatography| Chapter 4 | Challenges and Advances in Pharmaceutical Research Vol. 9

 The current work discusses developing a novel method for estimating residual solvents in gliclazide using gas chromatography and determining its consistency, reliability, and reproducibility through validation. A Gas chromatograph equipped with a flame ionization detector, column DB-624 (60 m x 0.32 mm x 1.8 µm) with Nitrogen as carrier gas was used and the column temperature was 40°C (hold for 15 mins) and increased to 240°C at 20°C per min. According to the protocol, the solutions were made using N-Methyl-2-Pyrrolidone (NMP) diluent and suitably administered in the order specified. System appropriateness, Specificity, Linearity and Range, Accuracy, Precision, Limit of Detection, Limit of Quantitation, Ruggedness and Robustness were the validation parameters examined. Each validation parameter's test data has been compiled and documented. It was discovered that each parameter's results were combined with the specified acceptance criteria. As a result, the established method was regarded as reproducible, reliable, and consistent. The analysis method was determined to be dependable, consistent, and reproducible. It conforms with all parameters examined.

Author(s) Details:

Burhanuddin Madriwala,
Department of Pharmaceutical Chemistry, M.S. Ramaiah University of Applied Sciences, Bengaluru - 560054, Karnataka, India.

Judy Jays,
Department of Pharmaceutical Chemistry, M.S. Ramaiah University of Applied Sciences, Bengaluru - 560054, Karnataka, India.

Please see the link here: https://stm.bookpi.org/CAPR-V9/article/view/8673

The Validation of Immunoblot Sds-Page as a Qualitative and Quantitative Method for the Determination of Urinary Cystatin C Inneonates | Chapter 4 | Highlights on Medicine and Medical Research Vol. 8

 The first paragraph is an introduction. The quantitative determination of urinary Cystatin C (cyst-C) in conjunction with the qualitative study of its polymorphisms is an excellent tool for detecting newborns who are predisposed to renal function deficiency early on. The immunometric methods PETIA, PENIA, and EIA are used to quantify cyst-C in human biologic fluid, but they have limitations and do not allow for qualitative study. The aim of this study is to prove that Immunoblot SDS-PAGE can be used to analyse urinary cyst-C in both qualitative and quantitative ways. Urine was obtained from newborns in the S. Maria della Misericordia Hospital nursey. The immunoblot SDS-PAGE and optical density reading were used to investigate urinary cyst-C.

The qualitative analysis revealed two molecular forms: a reactivity around 70 KDa in all samples and a reactivity around 13 KDa in a small number of samples. This research helps researchers to link cyst-C polymorphisms to specific changes in renal function in newborns. The quantitative analysis is targeted, sensitive, and precise.

In reality, the assay precision and accuracy coefficients of variance were both 10%, the detection limit was 0.009 ng/L, and the calibration line had adequate linearity (range 0.02-0.3 ng/L). Also without the use of protease inhibitors, the stability of urinary cyst-C was sufficient as long as the assay was performed on newly recruited urine or immediately after thawing samples that had been frozen for up to six months.

Conclusion: Immunoblot SDS-PAGE study of urinary cyst-C is a reliable tool for obtaining a qualitative and quantitative analysis. This method reveals previously unknown knowledge about a 70 KDa cyst-C shape. The assay could provide diagnostic information that isn't accessible through immunometric methods.

Author (s) Details

C. Grasselli
Department of Surgical and Biomedical Sciences, Section of Obstetrics and Gynecology, University of Perugia, Perugia, Italy.

A. Barbati
Department of Surgical and Biomedical Sciences, Section of Obstetrics and Gynecology, University of Perugia, Perugia, Italy.

L. Cesarini
Department of Chemistry, Biology and Biotechnology, University of Perugia, Perugia, Italy.

R. Pellegrino
Department of Chemistry, Biology and Biotechnology, University of Perugia, Perugia, Italy.

G. C. Di Renzo
Department of Surgical and Biomedical Sciences, Section of Obstetrics and Gynecology, University of Perugia, Perugia, Italy and GEBISA, Research Foundation, Perugia, Italy.

View Book :- https://stm.bookpi.org/HMMR-V8/article/view/821