Development and Validation of Sensitive GC and GC-MS Methods for the Detection and Quantification of Alkyl Mesylates in Pharmaceutical Active Ingredients | Chapter 8 | Recent Developments in Chemistry and Biochemistry Research Vol. 6

Methyl, ethyl, isopropyl, and hexyl mesylates were determined at trace levels in various active pharmaceutical ingredients by the capillary gas chromatographic method using flame ionization and mass spectrometers as detectors because of their mutagenic, carcinogenic, and teratogenic potential health risks in the medicines consumed by humans. A wide-bore gas chromatographic capillary column, the DB-WAX column (30 m × 0.53 mm × 1.0 µ m), was used for method development and validation. The carrier gas is helium for GC and GCMS methods with an injection volume of 4 µ L. Standard and sample solutions were prepared in a non-polar solvent such as n-hexane with the help of the solid-liquid extraction technique. The detection and quantitation limits were 0.02 and 0.05 ppm for methyl, ethyl, isopropyl, and hexyl mesylates for the GC and GCMS methods were achieved at very low levels by enhancing the analyte concentration up to 1 g quantity. The method was validated as per the procedures provided by the International Council for Harmonization of Technical Requirements for Pharmaceuticals for Human Use (ICH) and the Food and Drug Administration (FDA) of the United States of America. The %RSD for methyl, ethyl, isopropyl, and hexyl mesylates were less than 2.5%. The linearity of the method was demonstrated from 0.02 ppm to 5 ppm with respect to the analyte concentration, and it afforded correlation coefficients exceeding 0.99. The recoveries of methyl mesylate, ethyl mesylate, isopropyl mesylate, and hexyl mesylate were in the range of 97.1 to 107.1%. Hence, this is a robust method for the determination of alkyl mesylates in these APIs. Also, this method has been verified by a gas chromatograph equipped with mass spectrometry (GC-MS) for the detection of alkyl mesylates.

 

Author (s) Details

N Balaji
Analytical Development Laboratory, Apicore LLC, New Jersey, USA.

 

Sayeeda Sultana
Department of Chemistry, St. Peter’s University, Avadi, Chennai, Tamil Nadu, India.

 

Please see the book here:- https://doi.org/10.9734/bpi/rdcbr/v6/2320

 

Stability Indicating UV Spectrophotometric Method Development and Validation of Fisetin in Pure and Pharmaceutical Capsule Dosage Form | Chapter 2 | Pharmaceutical Research: Recent Advances and Trends Vol. 2

 

Objective: The objective of the study was to develop and UV Spectrophotometric method and apply the method to dosage form.

Methods: A simple, precise and sensitive ultraviolet spectrophotometric method was developed for the determination of Fisetin in pure and pharmaceutical capsule dosage form; the spectroscopic method was run through Shimadzu UV-1800 with solvent of Methanol: 0.1%OPA was used in this method-working wavelength was selected at 362nm.

Results: Beer-Lambert’s law revealed a good correlation in the concentration range of 3-15µg/ml. The absorbance was found to be 0.385 with %RSD for interday precision and intraday Precision was 0.53% & 0.51%.

Conclusion: The developed method was successfully applied to the determination of Fisetin in commercially available dosage forms. A statistical comparison of the results showed an insignificant difference between the proposed method and reference method. The proposed methods offered the advantages of simplicity and economy that can be applied without the need for expensive instrumentation and reagents in quality control analysis.

 

Author(s)details:-

 

R. Nageswara Rao
Department of Pharmaceutical Analysis, Santhiram College of Pharmacy, Nandyal-518501, Andhra Pradesh, India.

 

L. Siva Shankar Reddy
Department of Pharmaceutical Analysis, Santhiram College of Pharmacy, Nandyal-518501, Andhra Pradesh, India.

 

N. Madangopal
Department of Pharmaceutical Analysis, Santhiram College of Pharmacy, Nandyal-518501, Andhra Pradesh, India.

 

M Lakshmi Devi
Department of Pharmaceutical Analysis, Santhiram College of Pharmacy, Nandyal-518501, Andhra Pradesh, India.

R. Dharani
Department of Pharmaceutical Analysis, Santhiram College of Pharmacy, Nandyal-518501, Andhra Pradesh, India.

 

K. Raj Kumar
Department of Pharmaceutical Analysis, Santhiram College of Pharmacy, Nandyal-518501, Andhra Pradesh, India.

 

N. Venkateswara Reddy
Department of Pharmaceutical Analysis, Santhiram College of Pharmacy, Nandyal-518501, Andhra Pradesh, India.

 

P. Chandana
Department of Pharmaceutical Analysis, Santhiram College of Pharmacy, Nandyal-518501, Andhra Pradesh, India.

 

V. Ravikumar
Department of Pharmaceutical Biotechnology, School of Pharmacy, Guru Nanak Institutions Technical Campus, Hyderabad, Telangana, India.

 

J. Kumar Raja
Department of Pharmaceutical Analysis, Mother Teresa College of Pharmacy, Kothuru, Sanketika Nagar, Sathupally, Telangana 507303, India.

 

Please See the book here :-  https://doi.org/10.9734/bpi/prrat/v2/563

Bioanalytical Method Development and Validation of Garenoxacin Mesylate in Human Plasma by RP-HPLC and Its Pharmacokinetic Application | Chapter 9 | Advanced Concepts in Pharmaceutical Research Vol. 7

A simple, precise, accurate RP-HPLC method was developed for the estimation of Garenoxacin mesylate in human plasma using Ciprofloxacin Hydrochloride as an internal standard. The chromatographic conditions optimized were Zorbax Eclipse XDB C18 (250 x 4.6 mm, 5µ) column, Mobile phase 0.1% OrthoPhosphoric Acid and Acetonitrile in the ratio of 50:50 (% v/v) with a flow rate of 1.0 ml/min and injection volume of 50 µL. The detection wavelength was set to 240 nm with a column temperature of 30°C. The retention time of Garenoxacin mesylate was found to be 4.0 min. % Coefficient of Variation of Garenoxacin mesylate was found to be 4.30. % Recovery was obtained as 98.97%. The linearity of the proposed method was established in the concentration range of 0.04 to 4 µg/ml (Correlation Coefficient = 0.999). The lower limit of quantification was 0.04 µg/ml which reached the level of a drug possibly found in human plasma. Further, the reported method was validated as per the ICH guidelines and found to be well within the acceptable range. The method was successfully applied to a pharmacokinetic study after oral administration of immediate-release Zinox tablets (200 mg) in healthy Albino rabbits. The mean Cmax was found to be 5540 ng/ml, which occurred at a Tmax of 1.00 hr. The half-life and AUC0-α values were found to be 13.52 hr and 72187 ng. hr/ml. The method was found to be applicable to bioequivalence studies.

Author(s) Details:

A. Ajitha,
Department of Pharmaceutical Chemistry, Faculty of Pharmacy, Sri Ramachandra Institute of Higher Education and Research (Deemed to be University), No.1 Ramachandra Nagar, Porur, Chennai - 600 116, India.

K. Sujatha,
Department of Pharmaceutical Chemistry, Faculty of Pharmacy, Sri Ramachandra Institute of Higher Education and Research (Deemed to be University), No.1 Ramachandra Nagar, Porur, Chennai - 600 116, India.

Please see the link here: https://stm.bookpi.org/ACPR-V7/article/view/13733

Spectrophotometric Method for Determination of Azelaic Acid: Development and Validation Approach | Chapter 17 | Advanced Concepts in Pharmaceutical Research Vol. 3

 This phase evaluates to develop accurate, plain, UV spectrophotometric method which is empty extraction techniques, and smaller time and highly delicate technique. This study illustrates a simple, accurate, exact and cost effective UV-visible spectrophotometric plan for the estimation of Azelaic acid in pure and drug formulations. The analytically useful working groups in Azelaic acid have not been adequately exploited for designing appropriate, visible spectrophotometric methods accordingly still offer a scope to expand more visible spectrophotometric methods accompanying better sensitivity, selectivity, accuracy and accuracy. The method is established the measurement of absorbance of Azelaic acid solution in Phosphate safeguard pH 6.8 at 204nm in the wavelength range of 200-400nm. When using sure media and concentration ranges of 10–50µ g/ml, the process complies with Beer’s Lambert’s standard. Calculations were still performed for the slope, intercept, and equivalence coefficient. The presence of coarse excipients in tablets did not impair the process, according to the results of the percentage improvement investigation. In accordance with the approvals set forth by the Worldwide Conference on Harmonization (ICH), determinants such as extent of object, precision, accuracy, and feeling studies, which includes limit of discovery and limit of quantitation, were examined. The proposed form was found to be natural, accurate, precise and expeditious for the routine determination of Azelaic acid in pure and drug formulation.

Author(s) Details:

T. V. Kadam,
Department of Pharmaceutics, KVN Naik SPS's Institute of Pharmaceutical Education and Research, Canada Corner, Nashik, India.

A. B. Darekar,
Department of Pharmaceutics, KVN Naik SPS's Institute of Pharmaceutical Education and Research, Canada Corner, Nashik, India.

Please see the link here: https://stm.bookpi.org/ACPR-V3/article/view/12769

Development and Validation of HPLC Assay Method of Tofisopam by QBD Approach | Chapter 6 | Novel Aspects on Pharmaceutical Research Vol. 8

The aim of the work is to develop and confirm novel, simple, increased reversed phase chromatography form for assay of Tofisopam in pure and pill form. Quality by design (QBD) refers to the achievement of sure predictable character with desired and fixed specifications. The QbD approach stresses product and process understanding with character risk management and controls, happening in higher assurance of crop quality, regulatory elasticity, and continual bettering. The experimental trial was by Box Behnken design using Design Expert® program 10 version. The attributes picked were peak symmetry, NTP and peak purity. The forecasted data compensated with actual exploratory data. The exploratory design suggested the robust MODR domain for the TF HPLC method development. All the approved parameters were inside the acceptable criteria of ICH directions. The optimized chromatographic environments required quaternary send with travelling phase of Water: Acetonitrile 25:75 v/v at 1 ml/min, microwave temperature at 25oC at 310 nm utilizing C18 (250 X 4.6 mm Id, 5μm) column and PDA detector accompanying a run time of 5 brief time period. In this investigation, three independent variables-peak proportion, retention time, and NTP-were used to decide the concentration of the natural phase, oven hotness, and flow rate. The linearity design, precision, accuracy, and precision were all verified. With an overall average veracity of 99.98%, the approach provided linear reactions spanning the aggregation range of 4 to 24 ppm. Regarding the tofisopam retention time, the approach was trustworthy, repeatable, and precise.

Author(s) Details:

Megha Kokane,
Department of Quality Assurance, Shri. D. D. Vispute College of Pharmacy & Research Center, New Panvel, Navi Mumbai-410206, Maharashtra, India.

Jeeja Pananchery,
Department of Pharmacognosy, D. Y. Patil Deemed to be University School of Pharmacy, Nerul, Navi Mumbai-400507, Maharashtra, India.

Monika Jadhav,
Department of Quality Assurance, C. U. Shah College of Pharmacy, SNDT Women’s University, Sir Vithaldas Thakersay, Santacruz West, Juhu, Mumbai-400049, Maharashtra, India.

Ashish Jain,
Shri. D. D. Vispute College of Pharmacy & Research Center, New Panvel, Navi Mumbai-410206, Maharashtra, India.

Please see the link here: https://stm.bookpi.org/NAPR-V8/article/view/11653

First and Second Order Derivative Spectrophotometric Methods for Simultaneous Determination of Emtricitabine and Tenofovir Disoproxil Fumarate Tablets | Chapter 5 | Progress in Chemical Science Research Vol. 9

 Emtricitabine and tenofovir disoproxil fumarate in clean and tablet quantity forms are together estimated utilizing first and second order derivative spectrophotometric designs devised in the current study. Emtricitabine and tenofovir disoproxil Fumarate were linked to create a standard/sample, and the ranges of the incorporation, first order, and second order derivatives were written distinguished to a reagent blank. With absorbance principles of 0.639, 0.420, and 0.164, respectively, three peaks at 265 and 215 nm and individual lowland at 235 nm were noted in the incorporation spectra. In the first order derivative range, three definite peaks at 380, 325, and 260 nm and three negative peaks at 355, 280, and 225 nm were identified. The peak at 260 nm and the basin at 280 nm have the chief positive and negative amplitudes, individually, compared to the different highs and lows.  In the second order derivative spectrum, three peaks at 365, 290 and 250 nm accompanying best positive size at 250 nm and three valleys at 350, 265 and 215 nm accompanying maximum negative size at 215 nm were noted. In order to substantiate the approach for tenofovir disoproxil fumarate and emtricitabine, certain amplitudes at 282.4 nm and negative amplitudes at 258.7 nm in the combined first derivative range, respectively, were calculated.  Emtricitabine was ratified using the size of the second derivative sharp peak at 282.4 nm in the case of the second derivative pattern. Emtricitabine interferes with calculations of tenofovir disoproxil Fumarate at 258.7 nm, so the difference 'tween two together amplitudes was used to validate the procedure for tenofovir disoproxil Fumarate. System and procedure accuracy RSD percentages were raise to be inside satisfactory bounds. Accuracy trials at three spiking levels designated that the mean recovery allotment categorized from 99.4 to 100.48.  The proposed plans were used to decide the Truvada assay, and it was discovered that the allotment of assay for emtricitabine and tenofovir disoproxil Fumarate, respectively, was in the range of 100.75 ± 0.534 and 99.46 ± 0.671.   The grown plans were found expected exact, accurate, undeviating and sensitive.

Author(s) Details:

B. Valli Purnima,
Department of Chemistry, Acharya Nagarjuna University, Guntur, India and Department of Chemistry, Sir C. R. Reddy College for Women, Vatluru, Eluru, India.

G. Ramu,
Department of Chemistry, Sir C. R. Reddy College-Autonomous, Eluru, India.

D. Ramachandran,
Department of Chemistry, Acharya Nagarjuna University, Guntur, India.

Please see the link here: https://stm.bookpi.org/PCSR-V9/article/view/10699

LC and LC-MS/MS Studies for the Characterization of Forced Degradation Products of Tucatinib, a Novel Tyrosine Kinase Inhibitor| Chapter 3 | Challenges and Advances in Pharmaceutical Research Vol. 10

 The happening, validation, and characterisation of compulsory degradation products utilising LC-MS/MS were the main aims of the current investigation.Using an isocratic HPLC approach, tucatinib maybe measured quantitatively at a awareness of 239 nm in a simple, selective, substantiated, and well-defined method. An isocratic elution of samples was performed on an Inertsil ODS (250x4.6mm, 5m) procession with a mobile aspect of 70:30v/v Acetonitrile and formic acid (0.1%) delivered at a flow rate of 1.0 mL/brief time period. The degradation amount created during the strained degradation inquiry were characterised using MS/MS. Over the aggregation range of 5-100μg/ml, a good linear answer was obtained. Tucatinib's LOD and LOQ were determined expected 0.05 and 0.5, respectively. The approach was quantitatively determined in terms of order appropriateness, linearity, accuracy, accuracy, and strength in accordance with standard directions, and the findings were found expected within satisfactory limits. In studies on forced degeneration, the medication decomposed in sour, alkaline, and decline environments. It was persistent that the approach could be used for standard tucatinib study. Since there hasn't happened any evidence of an LC-MS/MS design for quantifying tucatinib and its degradation fruit in the literature. A device for researching the complete tucatinib degradation process has to be grown.

Author(s) Details:

S. K. Reehana,
Department of Pharmaceutical Analysis, University College of Pharmaceutical Sciences, Acharya Nagarjuna University; Nagarjuna Nagar, Guntur – 522510, Andhra Pradesh, India.

K. Sujana,
Department of Pharmaceutical Analysis, University College of Pharmaceutical Sciences, Acharya Nagarjuna University; Nagarjuna Nagar, Guntur – 522510, Andhra Pradesh, India.

A. Suneetha,
Department of Pharmaceutical Analysis, KVSR Siddhartha College of Pharmaceutical Sciences; Vijayawada – 520010, Andhra Pradesh, India.

Please see the link here: https://stm.bookpi.org/CAPR-V10/article/view/8797

Validation, Quantification and Stress Degradation Studies of Lenvatinib Mesylate in Bulk Drug and Pharmaceutical Dosage Forms Using Ultra Performance Liquid Chromatography| Chapter 3 | Current Aspects in Pharmaceutical Research and Development Vol.9

 The goal of this work was to use UPLC to establish a new method for quantifying Lenvatinib mesylate in bulk drug and pharmaceutical dose form, as well as to validate the method and conduct stress degradation experiments on the drug.

UPLC HSS C18 (100 mm x 2.1mm, 1.8m) column, mixture of 0.1 percent OPA and Acetonitrile (50:50) mobile phase run on an isocratic mode at a flow rate of 0.3ml/min, 240nm detection wavelength, and column oven temperature maintained at 30oC were the optimised chromatographic conditions for drug elution.

Lenvatinib's retention time was found to be 1.24 minutes. In compliance with ICH requirements, the suggested method was validated for several validation parameters. In the concentration range of 2.5g/ml – 15g/ml, the technique followed Beer's law with a correlation coefficient of 0.9996. The percent RSD and percent recovery, respectively, were found to be 0.4 and 99.66 percent – 100.30 percent. It was discovered that the procedure was accurate, precise, particular, linear, rugged, and robust. The medication was subjected to a variety of stress conditions, including acidic, basic, peroxide, neutral, photolytic, and thermal. The net degradation was found to be within acceptable bounds.

Conclusion: The devised approach for estimating Lenvatinib in pharmaceutical dosage form can be used for routine analysis.

Author(s) Details:

Jahnavi Bandla,
Department of Pharmaceutical Analysis and QA, Faculty of Pharmacy, Vishnu Institute of Pharmaceutical Education and Research, Narsapur, Medak-502313, Telangana, India.

S. Ganapaty,
Department of Pharmacognosy and Phytochemistry, GITAM Institute of Pharmacy GITAM University, Rushikonda, Visakhapatnam-530045, Andhra Pradesh, India.

Please see the link here: https://stm.bookpi.org/CAPRD-V9/article/view/5963#