This study is done to access the chemical stability of the candidate compound in the pharmaceuticals.
Usually, it is performed at the preliminary stage in the process of drug development. Forced degradation/ stress
testing is performed under accelerated environment. The experimental conditions cause the candidate compound
to degrade under extreme conditions like acid and base hydrolysis, peroxide oxidation, photo-oxidation and
thermal stability to identify the resultant degradation products. This helps to establish degradation pathways and
thus intrinsic stability of a drug substance. The stability of product describes shelf life and storage conditions and
helps in the selection of appropriate formulations and their suitable packaging. This is compulsory for regulatory
documentation. The commonly used analytical approach for FDS is HPLC with UV and/ or MS but these
techniques consume a lot of time and not provide high resolution to confirm the precise detection of degradation
products. Use of UPLC with photodiode array and MS analysis supports the identification of degradation
products and also reduces the time needed to evolve stability indicating methods.
Method Development and Validation on Etomidate injection by RP-HPLC
This document describes the development and validation of a high performance liquid chromatography (HPLC) method for the analysis of etomidate injection. The method uses a Waters HPLC system with a Develosil-ODS-UG column and a mobile phase of acetonitrile and phosphate buffer at a ratio of 40:60. The method was validated per ICH guidelines and found to be accurate, precise, linear, robust and sensitive for quantifying etomidate in injections. The method was then applied to analyze etomidate levels in marketed injection formulations.
Development and Validation of a Spectrophotometric method using Vierordt’s Me...
Objective: The objective of the current study was to develop rapid, accurate, reproducible, validated and economical Vierordt’s Method for the simultaneous determination of CEF and MOX in tablet dosage forms. Method: This method of analysis was based upon the absorption of drugs at wavelength maximum of each other. Two wavelengths of 289.10 and 295.10 nm were selected which are the λmax of two drugs for the development of the simultaneous equations. The absorbance of CEF and MOX were measured and the absorptivity values were determined at all the two selected wavelengths. Result & Discussion: The linearity was found to be 3-9µg/ml for CEF & MOX respectively. Recovery was in the range of 98 –102%; the values of standard deviation and% R.S.D. were found to be <2% shows the high accuracy of the method. The Limit of Detection and Limit of Quantitation were theoretically calculated which were found to be 0.0224 and 0.0678 for CEF and 0.0070 and 0.0214 for MOX respectively. Robustness and Ruggedness were also carried out and percentage RSD was found to be less than 2.0 %. The assay of Cefixime and Moxifloxacin was found to be 99.36% and 98.75%.The proposed method has been validated as per ICH guidelines and successfully applied to the estimation of CEF and MOX in their combined Tablet dosage form.
1. A new RP-HPLC method was developed and validated for the estimation of Clopidogrel bisulphate in bulk drug and pharmaceutical formulations.
2. The method involved using a C18 column, mobile phase of acetonitrile and phosphate buffer at a ratio of 60:40, and detection at 224 nm.
3. The method was found to be linear, precise, accurate, specific, robust and suitable for the routine analysis of Clopidogrel bisulphate in quality control labs.
Head space gas_chromatography_analysis_of_residual (1)DivvyaIndran
This document describes a study that developed and validated a gas chromatography method for simultaneously analyzing 16 residual solvents using an EC-5 column with headspace injection. The method was found to provide good separation and resolution between peaks. Key findings include:
- The EC-5 column was selected based on matching solute and stationary phase polarities to improve resolution.
- The method was validated according to ICH guidelines and showed the method to be specific, accurate, precise, and rugged.
- The retention times of the 16 solvents were reported and resolution between peaks was calculated, demonstrating good separation of the solvents.
The IOSR Journal of Pharmacy (IOSRPHR) is an open access online & offline peer reviewed international journal, which publishes innovative research papers, reviews, mini-reviews, short communications and notes dealing with Pharmaceutical Sciences( Pharmaceutical Technology, Pharmaceutics, Biopharmaceutics, Pharmacokinetics, Pharmaceutical/Medicinal Chemistry, Computational Chemistry and Molecular Drug Design, Pharmacognosy & Phytochemistry, Pharmacology, Pharmaceutical Analysis, Pharmacy Practice, Clinical and Hospital Pharmacy, Cell Biology, Genomics and Proteomics, Pharmacogenomics, Bioinformatics and Biotechnology of Pharmaceutical Interest........more details on Aim & Scope).
All manuscripts are subject to rapid peer review. Those of high quality (not previously published and not under consideration for publication in another journal) will be published without delay.
This document describes the development and validation of a spectrophotometric method for the determination of the antiepileptic drug rufinamide in bulk and pharmaceutical formulations. Rufinamide forms a colored complex with the dye bromocresol green under acidic conditions that can be extracted with chloroform and measured spectrophotometrically. The method was optimized and validated according to ICH guidelines, demonstrating good linearity, precision, accuracy, and sensitivity for quantifying rufinamide concentrations between 10-50 μg/mL. The method was successfully applied to analyze rufinamide levels in commercial tablet formulations, indicating it is suitable for the routine analysis of this drug in quality control testing.
Method Development and Validation on Etomidate injection by RP-HPLCpharmaindexing
This document describes the development and validation of a high performance liquid chromatography (HPLC) method for the analysis of etomidate injection. The method uses a Waters HPLC system with a Develosil-ODS-UG column and a mobile phase of acetonitrile and phosphate buffer at a ratio of 40:60. The method was validated per ICH guidelines and found to be accurate, precise, linear, robust and sensitive for quantifying etomidate in injections. The method was then applied to analyze etomidate levels in marketed injection formulations.
Development and Validation of a Spectrophotometric method using Vierordt’s Me...SriramNagarajan19
Objective: The objective of the current study was to develop rapid, accurate, reproducible, validated and economical Vierordt’s Method for the simultaneous determination of CEF and MOX in tablet dosage forms. Method: This method of analysis was based upon the absorption of drugs at wavelength maximum of each other. Two wavelengths of 289.10 and 295.10 nm were selected which are the λmax of two drugs for the development of the simultaneous equations. The absorbance of CEF and MOX were measured and the absorptivity values were determined at all the two selected wavelengths. Result & Discussion: The linearity was found to be 3-9µg/ml for CEF & MOX respectively. Recovery was in the range of 98 –102%; the values of standard deviation and% R.S.D. were found to be <2% shows the high accuracy of the method. The Limit of Detection and Limit of Quantitation were theoretically calculated which were found to be 0.0224 and 0.0678 for CEF and 0.0070 and 0.0214 for MOX respectively. Robustness and Ruggedness were also carried out and percentage RSD was found to be less than 2.0 %. The assay of Cefixime and Moxifloxacin was found to be 99.36% and 98.75%.The proposed method has been validated as per ICH guidelines and successfully applied to the estimation of CEF and MOX in their combined Tablet dosage form.
1. A new RP-HPLC method was developed and validated for the estimation of Clopidogrel bisulphate in bulk drug and pharmaceutical formulations.
2. The method involved using a C18 column, mobile phase of acetonitrile and phosphate buffer at a ratio of 60:40, and detection at 224 nm.
3. The method was found to be linear, precise, accurate, specific, robust and suitable for the routine analysis of Clopidogrel bisulphate in quality control labs.
Method Development and Validation of Clopidogrel Bisulphate by Reverse Phase-...SriramNagarajan15
A new, simple sensitive, rapid, accurate and precise RP-HPLC method was developed for the estimation of Clopidogrel bisulphate in bulk drug and pharmaceutical formulation. Clopidogrel bisulphate was chromatographed on a reverse phase C18column (150 mm x 4.5 mm, i.d 5μm) in a mobile phase consisting of acetonitrile and phosphate buffer (pH: 3.0) in the ratio of 60:40 % v/v. The mobile phase was pumped at a flow rate of 1 ml/min with detection at 224 nm. The detector response was linear in the concentration of 50-150 μg /ml. The limit of detection and limit of quantitation was found to be 1.3 and 4.2 µg/ml, respectively. The intra and inter day variation was found to be less than 2%. The mean recovery of the drug from the solution was 99.79%. The proposed method is simple, fast, accurate, precise and reproducible hence, it can be applied for routine quality control analysis of Clopidogrel bisulphate in bulk drug and pharmaceutical formulation. Key words: Clopidogrel bisulphate, RP-HPLC, Validation, Accuracy, Precision.
Spectrophotometric Determination of Drugs and Pharmaceuticals by Cerium (IV) ...IOSR Journals
Simple, sensitive, accurate, and precise spectrophotometric methods for quantitative determination of drugs, viz., Darifenacin (DAR), Esmolol Hydrochloride (ESM), Montelukast Sodium (MON), Sildenafil citrate (SIL),Terbinafine (TER) and Tramadol Hydrochloride (TRA) were developed. The method of each drug depends upon oxidation of drugs by Ce (IV) (Excess) and estimating the amount of unreacted Ce (IV) by amaranth dye at 523nm. The calibration curves obeyed Beer’s law over the concentration range of 1.4-7.0 μg ml-1 (DAR), 2-14 μg ml-1 (ESM), 2-10 μg ml-1 (MON), 20-70 μg ml-1 (SIL), 3-21 μg ml-1 (TER) & 2-14 μg ml-1 (TRA). The methods have been validated in terms of guidelines of ICH and applied to analysis of pharmaceuticals.
Determination of Riociguat by Oxidative Coupling Using Visible SpectrophotometryRatnakaram Venkata Nadh
This document describes a simple spectrophotometric method developed to determine the drug riociguat in bulk and tablet formulations. The method is based on the oxidation of MBTH by Fe+3 ions in acidic medium, which forms an active coupling species. This species then couples with riociguat to form a chromophore with a maximum absorption at 660 nm. The method was validated according to ICH guidelines and showed good linearity, reproducibility, accuracy, and precision for the determination of riociguat.
This document describes methods for the quantitative determination and analysis of Promethazine Hydrochloride and Prasugrel Hydrochloride using Folin-Ciocalteu reagent (FCR) through spectrophotometric studies. Calibration curves were constructed for both drugs using FCR and results were validated in terms of limits of detection, quantification, accuracy and precision. The developed methods were applied to pharmaceutical formulations containing the drugs and found to give satisfactory recoveries. Various factors affecting the absorbance were also optimized.
Simultaneous estimation of metformin hydrochloride and glibenclamide by rphpl...IJSIT Editor
A high performance reverse phase liquid chromatographic procedure is developed for simultaneous
estimation of Metformin hydrochloride and Glibenclamide in combined tablet dosage form. The method was carried
out on a Agilent Hypersil ODS (25cm x 4.6mm, i.d. 5µ) column with a mobile phase used consisting of acetonitrile:
mono basic sodium phosphate Buffer (50:50) and the pH of buffer was adjusted to 2.5 using 2M Orthophosphoric acid.
The detection of the combined dosage form was carried out at 228 nm and a flow rate employed was 1 ml/min and
column oven temperature at 300C. The retention times of Metformin HCl & Glibenclamide were 2.709& 9.216 minutes
respectively. The developed method was validated in terms of accuracy, precision, linearity, limit of detection, limit of
quantification as per ICH norms. The proposed method can be used for the estimation of these combined drugs.
Quality-by-design-based development and validation of a stability-indicating ...Ratnakaram Venkata Nadh
A systematic design-of-experiments was performed by applying quality-by-design concepts to determine
design space for rapid quantification of teriflunomide by the ultraperformance liquid chromatography
(UPLC) method in the presence of degradation products. Response surface and central composite
quadratic were used for statistical evaluation of experimental data using a Design-Expert software. The
response variables such as resolution, retention time, and peak tailing were analyzed statistically for the
screening of suitable chromatographic conditions. During this process, various plots such as perturbation,
contour, 3D, and design space were studied. The method was developed through UPLC BEH C18
2.1 � 100 mm, 1.7-μ column, mobile phase comprised of buffer (5 mM K2HPO4 containing 0.1%
triethylamine, pH 6.8), and acetonitrile (40:60 v/v), the flow rate of 0.5 mL min 1 and UV detection at
250 nm. The method was developed with a short run time of 1 min. Forced degradation studies revealed
that the method was stability-indicating, suitable for both assay and in-vitro dissolution of a drug product.
The method was found to be linear in the range of 28–84 μg mL 1, 2.8–22.7 μg mL 1 with a correlation
coefficient of 0.9999 and 1.000 for assay and dissolution, respectively. The recovery values were found in
the range of 100.1–101.7%. The method was validated according to ICH guidelines.
Spectrophotometric Determination of Cardiovascular DrugsIJMER
International Journal of Modern Engineering Research (IJMER) is Peer reviewed, online Journal. It serves as an international archival forum of scholarly research related to engineering and science education.
Spectrophotometric Oxidation Method for the Determination of Teneligliptin by...ijtsrd
A sensitive, precise, accurate, simple and rapid spectrophotometric method has been developed for the estimation of Teneligliptin in pharmaceutical formulations and in the drug dosage form. During the course of study, it is observed that acidic solution of the drug formed the oxidation product with Bromate "“ Bromide mixture. This property of the drug is exploited for the development of spectrophotometric method for the determination and analysis of the drug. The oxidation product showed ?max at 250 nm. The linearity range for Teneligliptin is found to be 10 µgml to 250 µgml. Recovery studies gave satisfactory results indicating that none of common additives and excipients interfere the assay method. The molar absorptivity and the sandell sensitivity of the method are evaluated and the values are found to be to be 1.1645×104 lit molecm and 0.0366 µg mlcm2 respectively. I. Lakshmi Prasanna | G. T. Naidu | G. Abdul Huq"Spectrophotometric Oxidation Method for the Determination of Teneligliptin by Using Bromate "“ Bromide Mixture" Published in International Journal of Trend in Scientific Research and Development (ijtsrd), ISSN: 2456-6470, Volume-2 | Issue-5 , August 2018, URL: http://www.ijtsrd.com/papers/ijtsrd18253.pdf http://www.ijtsrd.com/physics/other/18253/spectrophotometric-oxidation-method-for-the-determination-of-teneligliptin-by-using-bromate---bromide-mixture/i-lakshmi-prasanna
This document describes the development and validation of a stability-indicating RP-LC method for the determination of famciclovir (FCV) in the presence of its impurities and degradation products. A gradient reverse phase liquid chromatographic method was developed using an Inertsil ODS 3V column with a mobile phase of a potassium dihydrogen orthophosphate buffer and methanol mixture. FCV was subjected to oxidative, acid, base, hydrolytic, thermal, and photolytic degradation and was found to degrade significantly under oxidative, acid and base conditions. The developed method was validated according to ICH guidelines and demonstrated specificity, linearity, accuracy, precision, and robustness. This stability-indicating method can
This document describes a spectrofluorimetry method for determining nalidixic acid concentrations in human plasma. The method involves extracting nalidixic acid from plasma samples using chloroform and analyzing the samples using a spectrofluorimeter. The method was used to analyze plasma samples from a study comparing the bioavailability of a new generic nalidixic acid tablet formulation to a standard brand name formulation. Results of in vitro tests like dissolution and assay showed the new generic formulation was comparable to the standard. Pharmacokinetic analysis of plasma concentration data from subjects who received the formulations found no significant differences between the products.
Design of Pulsatile Tablets of Pantoprazole Sodium: Factorial Design ApproachReshma Fathima .K
This document describes a study that developed and optimized a pulsatile drug delivery system containing pantoprazole sodium using a 32 full factorial design approach. Six core tablets were initially prepared and evaluated. Amounts of microcrystalline cellulose (MCC) and sodium starch glycolate (SSG) were selected as independent variables in the factorial design to study their effects on tablet properties. The optimized core formulation (f3) was then coated with Eudragit S to produce pulsatile tablets. In vitro dissolution studies showed the coated tablets remained intact in acid media and released drug after reaching the intestine, indicating successful development of a pulsatile delivery system for pantoprazole sodium.
Formulation and Evaluation of Moxifloxacin Loaded Alginate Chitosan Nanoparti...pharmaindexing
This document describes the formulation and evaluation of moxifloxacin-loaded alginate-chitosan nanoparticles for treating tuberculosis. Moxifloxacin nanoparticles were prepared using an ionic gelation method with varying polymer ratios and drug concentrations. Formulation MF3, with a drug concentration of 50 mg, exhibited the highest encapsulation efficiency, drug loading, and rate of recovery. In vitro drug release from MF3 was sustained over 96 hours with no significant changes observed after 3 months of stability testing. Scanning electron microscopy confirmed the nanoparticles had a discrete spherical structure without aggregation.
This document describes the development and validation of a stability-indicating high-performance thin layer chromatography (HPTLC) method for the analysis of modafinil, both as a bulk drug and in tablet formulations. The method utilizes silica gel plates with an ethyl acetate, acetone and methanol mobile phase. Modafinil demonstrates good linearity, precision, accuracy and robustness within the method validation parameters. The method is also shown to distinguish modafinil from its degradation products formed under various stress conditions like acid and base hydrolysis, oxidation, photolysis and heat. The developed HPTLC method can be applied for the quantitative analysis and identification of modafinil in pharmaceutical formulations.
This document describes the development and validation of an HPLC method for the simultaneous determination of impurities and degradation products in Cardiazol. The method utilizes gradient elution on a C18 column with UV detection at 240nm. The method was validated according to ICH guidelines and found to be specific, sensitive, linear, precise and accurate for quantifying two known impurities (Impurities A and B) and unknown degradation products. The method can also distinguish Cardiazol from degradation products formed under various stress conditions like acid/base hydrolysis and oxidation.
This document describes the development and validation of a reverse phase high performance liquid chromatography (RP-HPLC) method for the estimation of the drug Zidovudine. The method was developed using a C18 column with a mobile phase of acetonitrile and water at a pH of 4.8. The method was validated according to ICH guidelines and showed good linearity, precision, accuracy, specificity, robustness and recovery. The proposed RP-HPLC method can be used for the routine analysis of Zidovudine in pharmaceutical formulations.
The document summarizes research into developing tamoxifen citrate-loaded nanoparticles using the biodegradable polymer PLGA for breast cancer treatment. PLGA nanoparticles containing tamoxifen citrate were prepared using emulsion solvent evaporation techniques. Process parameters like drug-polymer ratio and homogenization speed were optimized. Characterization studies showed the nanoparticles were spherical and smooth. In vitro drug release was evaluated over time, with release profiles varying by centrifugation speed. Drug loading efficiency ranged from 18.6-71.98%. The nanoparticles showed potential as a controlled drug delivery system for tamoxifen citrate.
Method development and validation of Sodium Cromoglycate sujatabhosale5
Here are the key steps in the sample preparation procedure for UV spectroscopy:
1. A standard stock solution of 100 μg/ml was prepared by dissolving 10 mg of drug in 100 ml of mobile phase (ACN:Water 80:20).
2. From the stock solution, 10 ml was pipetted and diluted to 100 ml with mobile phase to obtain a 10 μg/ml working standard solution.
3. Tablets/capsules were weighed and powdered. An amount of powder equivalent to 10 mg of drug was transferred to a 100 ml volumetric flask.
4. The powder was dissolved in mobile phase and sonicated for 15 minutes. The volume was made up to mark with mobile phase to obtain a
folic acid chitosan conjugate nanoparticle containing azithromycin for the tr...shivamgupta1083
The document presents a research proposal for developing folic acid-chitosan conjugate nanoparticles containing azithromycin for treating colorectal diseases. The objectives are to prepare drug-loaded conjugates with desired release characteristics and assess their targeting efficacy and bio-distribution. The plan involves preformulation studies, preparing the folic acid-chitosan conjugate, loading the conjugate with azithromycin, and characterizing the nanoparticles. In vitro and in vivo studies will evaluate particle properties, drug release, cytotoxicity, and the ability to treat colorectal inflammation in a rat model.
The document summarizes a study evaluating the dissolution behavior of 500mg Paracetamol tablets according to USP guidelines using the paddle method. The study found that 126.2% of the Paracetamol dissolved within 30 minutes, meeting the USP and BP standards of dissolving at least 80% within 30 minutes. The paddle apparatus and UV spectrophotometry were used to test six tablets and obtain dissolution profiles. The results indicate the tested Paracetamol tablets meet pharmacopeial standards for dissolution.
Visible Spectrophotometric Analysis Method of Sodium Metamizole in Tablets
The aim of this research was to exactly quantify pure sodium metamizole from tablets , using a
spectrophotometric analysis in Visible range. The method applied has been subjected to a validation protocol which consisted in analyzing the following parameters: linearity of the method, detection limit (LD) ,
quantitation limit (LQ), Sandell’s sensitivity, interference of excipients, stability of prepared solutions, method and system precision, accuracy of the method. Following actual dosing, pure sodium metamizole amount
in tablet of pharmaceutical was found to be 477.477 mg assigned to a percentage content of 95.495 %, very close to official declared amount (500 mg), with an maximum average percentage deviation of only 4.505 % from the official declared active substance content. This value was situated below the maximum admissible percentage deviation from stated active substance content (± 5%), established by Romanian Pharmacopoeia, X-th Edition rules.
Method Development and Validation of Naftopidil by Reverse Phase-HPLC in Bulk...SriramNagarajan15
A new simple, accurate, rapid and precise isocratic High performance liquid chromatographic (HPLC) method was developed and validated for the determination of Etomidate (ETO) injection. The Method employs Waters HPLC system on Develosil –ods-UG column (300 x 3.9 mm x 5µm) and flow rate of 1.5 mL/min with a load of 20 µL. Acetonitrile and Phosphate buffer was used as mobile phase in the composition of 40:60. The Detection was carried out at 254 nm. Linearity ranges for Etomidate was 40-240 µg/ml respectively. Retention Time of Etomidate was found to be 12.061 minutes respectively. Percent recovery study values of Etomidate were found to be within 98-102 %. This newly developed method was successfully utilized for the Quantitative estimation of Etomidate in injectables. This method was validated for accuracy, precision, linearity and Robustness as per ICH guidelines.
RP-HPLC method development and validation of ritonavir in bulk and pharmaceut...SriramNagarajan17
This document describes the development and validation of an RP-HPLC method for the quantification of the HIV protease inhibitor ritonavir (RIT) in bulk and pharmaceutical dosage forms. A simple isocratic RP-HPLC method was developed using a C18 column, mobile phase of 0.02M potassium dihydrogen phosphate buffer and acetonitrile (70:30 v/v), and detection at 237 nm. The method was validated per ICH guidelines and showed good linearity from 25-150 μg/mL, precision <0.5% RSD, accuracy of 99.3-100.6% recovery, and ability to quantify RIT in pharmaceutical tablets without interference from excipients.
Abstract:
The Chronopharmacotherapy the drug administration is synchronised with circadian rhythms Formulation development of Microspheres is more reliable formulation as compare to single type dosage formulation due to it avoids dose dumping, as per required drug release profile is achieved For microspheres many polymers are used such as albumin, gelatine, starch, Eudragit, Polyacrylamide (“PAM”) these material loading capacity is high. Micro sponges which are Spherical are called as micro-balloons. Due to its hollow structure it shows good floating properties. In these systems use of Carbon-dioxide (CO2) as gas generating system which are used for floating purpose. The objective of present investigation is to prepared and evaluate a floating pulsatile drug delivery system of Aceclofenac. The strategy adopted for microspheres containing Aceclofenac as a material were prepared by emulsion solvent diffusion technique. Drug and polymer were mixed in dichloromethane and ethanol at 1:1 ratio. The drug and polymer solution were poured in water 50% W/V polyvinyl alcohol maintained at 30-40 C and the solution was stir at 500rpm using mechanical stirrer, The microspheres obtain were washed repeatedly with water until free from poly vinyl alcohol. The developed formulations were evaluated yield of floating microspheres particle size and shape, drug entrapment efficiency in-vitro evolution of floating ability, in-vitro drug release study. On the basis of these evolution parameters it was found that optimised floating pulsatile release formulation F7 showed higher drug entrapment efficiency floating time 6.8 minutes and the drug and polymer 32 1:3 ratio the particle size was increased.
Key Words: Chronopharmacotherapy, Floating pulsatile drug delivery, Aceclofenac.
This study evaluated the cytotoxicity of pegylated nanoliposomal cisplatin on ovarian cancer cells. Methoxypolyethylene glycol propionaldehyde was synthesized and characterized. Nanoliposomes encapsulating cisplatin were prepared using the reverse phase evaporation method and characterized. The nanoliposomes had a mean diameter of 125 nm and negative zeta potential. Cytotoxicity tests on ovarian cancer cells showed the IC50 of nanoliposomal cisplatin was lower than free cisplatin, indicating the nanoliposomal formulation was more cytotoxic. This study demonstrates pegylated nanoliposomal cisplatin has potential as a more effective cisplatin delivery system for ovarian cancer treatment.
IOSR Journal of Pharmacy (IOSRPHR), www.iosrphr.org, call for paper, research...iosrphr_editor
IOSR Journal of Pharmacy (IOSRPHR), www.iosrphr.org, call for paper, research paper publishing, where to publish research paper, journal publishing, how to publish research paper, Call for research paper, international journal, publishing a paper, call for paper 2012, journal of pharmacy, how to get a research paper published, publishing a paper, publishing of journal, research and review articles, Pharmacy journal, International Journal of Pharmacy, hard copy of journal, hard copy of certificates, online Submission, where to publish research paper, journal publishing, international journal, publishing a paper
1) The document evaluates the effect of varying mole ratios of reactants on the yield of ceftriaxone sodium synthesis. Ceftriaxone sodium was synthesized by reacting 7-ACT and MAEM, then with sodium salt.
2) Testing showed that increasing the mole ratio of MAEM increased the yield up to a ratio of 1:2, where the yield was 72.17% and purity was 99.32%. However, further increasing the ratio did not increase yield.
3) The highest mole ratio of 1:2 produced the highest yield while maintaining high purity. This suggests that a 1:2 mole ratio of reactants could be optimal for industrial scale ceftriaxone sodium production.
IRJET - Simultaneous Estimation of Pregabalin and Methylcobalamin in a Ma...IRJET Journal
This document describes the development and validation of a novel gradient reverse phase HPLC method for the simultaneous estimation of Pregabalin and Methylcobalamin in a marketed formulation. The method utilizes a C18 column with a mobile phase of potassium dihydrogen phosphate buffer and methanol in a gradient mode. Pregabalin and Methylcobalamin were well separated with retention times of 4.792 minutes and 7.586 minutes, respectively. The method was validated for parameters such as specificity, accuracy, precision, linearity, robustness and forced degradation studies. The developed method provides a simple, precise and accurate way to analyze Pregabalin and Methylcobalamin in a single run.
In-vitro evaluation techniques of anticancer, anti oxidant, anti microbial ZakiyaUsmani
This document discusses various in vitro methods used to evaluate potential anti-cancer and antioxidant compounds, as well as antimicrobial activity. It describes cytotoxicity assays such as MTT, SRB, clonogenic assays and dye exclusion tests that are used to study anti-cancer activity against cell lines. Methods to evaluate antioxidant activity in vitro include DPPH radical scavenging, hydrogen peroxide and superoxide radical scavenging assays. Diffusion and dilution methods are discussed for determining antimicrobial activity of compounds in vitro prior to animal studies.
Similar to STUDY OF MPS UNDER STRESSED CONDITIONS (20)
Understanding the Impact and Challenges of Corona Crisis on Education Sector...vivatechijri
n the second week of March 2020, governments of all states in a country suddenly declared
shutting down of all colleges and schools for a temporary period of time as an immediate measure to stop the
spread of pandemic that is of novel corona virus. As the days pass by almost close to a month with no certainty
when they will again reopen. Due to pandemic like this an alarm bells have started sounding in the field of
education where a huge impact can be seen on teaching and learning process as well as on the entire education
sector in turn. The pandemic disruption like this is actually gave time to educators of today to really think about
the sector. Through the present research article, the author is highlighting on the possible impact of
coronavirus on education sector with the future challenges for education sector with possible suggestions.
LEADERSHIP ONLY CAN LEAD THE ORGANIZATION TOWARDS IMPROVEMENT AND DEVELOPMENT vivatechijri
This document discusses the importance of leadership in leading an organization towards improvement and development. It states that leadership is responsible for providing a clear vision and strategy to successfully achieve that vision. Effective leadership can impact the success of an organization by controlling its direction and motivating employees. Leadership is different from traditional management in that it guides employees towards organizational goals through open communication and motivation, rather than simply directing work. The paper concludes that only leadership can lead an organization to change according to its evolving environment, while management may simply follow old rules. Leadership is key to adapting to new market needs and trends.
The topic of assignment is a critical problem in mathematics and is further explored in the real
physical world. We try to implement a replacement method during this paper to solve assignment problems with
algorithm and solution steps. By using new method and computing by existing two methods, we analyse a
numerical example, also we compare the optimal solutions between this new method and two current methods. A
standardized technique, simple to use to solve assignment problems, may be the proposed method
Structural and Morphological Studies of Nano Composite Polymer Gel Electroly...vivatechijri
The document summarizes research on a nano composite polymer gel electrolyte containing SiO2 nanoparticles. Key points:
1. Polyvinylidene fluoride-co-hexafluoropropylene polymer was used as the base polymer mixed with propylene carbonate, magnesium perchlorate, and SiO2 nanoparticles to synthesize the nano composite polymer gel electrolyte.
2. The electrolyte was characterized using XRD, SEM, and FTIR which confirmed the homogeneous dispersion of SiO2 nanoparticles and increased amorphous nature of the electrolyte, enhancing its ion conductivity.
3. XRD showed decreased crystallinity and disappearance of polymer peaks upon addition of SiO2. SEM revealed
Theoretical study of two dimensional Nano sheet for gas sensing applicationvivatechijri
This study is focus on various two dimensional material for sensing various gases with theoretical
view for new research in gas sensing application. In this paper we review various two dimensional sheet such as
Graphene, Boron Nitride nanosheet, Mxene and their application in sensing various gases present in the
atmosphere.
METHODS FOR DETECTION OF COMMON ADULTERANTS IN FOODvivatechijri
Food is essential forliving. Food adulteration deceives consumers and can endanger their health. The
purpose of this document is to list common food adulterant methods commonly found in India. An adulterant is
a substance found in other substances such as food, cosmetics, pharmaceuticals, fuels, or other chemicals that
compromise the safety or effectiveness of that substance. The addition of adulterants is called adulteration. The
most common reason for adulteration is the use of undeclared materials by manufacturers that are cheaper than
the correct and declared ones. The adulterants can be harmful or reduce the effectiveness of the product, or
they can be harmless.
The novel ideas of being a entrepreneur is a key for everyone to get in the hustle, but developing a
idea from core requires a systematic plan, time management, time investment and most importantly client
attention. The Time required for developing may vary from idea to idea and strength of the team. Leadership to
build a team and manage the same throughout the peak of development is the main quality. Innovations and
Techniques to qualify the huddles is another aspect of Business Development and client Retention.
Innovation for supporting prosperity has for quite some time been a focus on numerous orders, including PC science, brain research, and human-PC connection. In any case, the meaning of prosperity isn't continuously clear and this has suggestions for how we plan for and evaluate advances that intend to cultivate it. Here, we talk about current meanings of prosperity and how it relates with and now and then is a result of self-amazing quality. We at that point center around how innovations can uphold prosperity through encounters of self-amazing quality, finishing with conceivable future bearings.
An Alternative to Hard Drives in the Coming Future:DNA-BASED DATA STORAGEvivatechijri
Demand for data storage is growing exponentially, but the capacity of existing storage media is not keeping up, there emerges a requirement for a storage medium with high capacity, high storage density, and possibility to face up to extreme environmental conditions. According to a research in 2018, every minute Google conducted 3.88 million searches, other people posted 49,000 photos on Instagram, sent 159,362,760 e-mails, tweeted 473,000 times and watched 4.33 million videos on YouTube. In 2020 it estimated a creation of 1.7 megabytes of knowledge per second per person globally, which translates to about 418 zettabytes during a single year. The magnetic or optical data-storage systems that currently hold this volume of 0s and 1s typically cannot last for quite a century. Running data centres takes vast amounts of energy. In short, we are close to have a substantial data-storage problem which will only become more severe over time. Deoxyribonucleic acid (DNA) are often potentially used for these purposes because it isn't much different from the traditional method utilized in a computer. DNA’s information density is notable, 215 petabytes or 215 million gigabytes of data can be stored in just one gram of DNA. First we can encode all data at a molecular level and then store it in a medium that will last for a while and not become out-dated just like floppy disks. Due to the improved techniques for reading and writing DNA, a rapid increase is observed in the amount of possible data storage in DNA.
The usage of chatbots has increased tremendously since past few years. A conversational interface is an interface that the user can interact with by means of a conversation. The conversation can occur by speech but also by text input. When a chatty interface uses text, it is also described as a chatbot or a conversational medium. During this study, the user experience factors of these so called chatbots were investigated. The prime objective is “to spot the state of the art in chatbot usability and applied human-computer interaction methodologies, to research the way to assess chatbots usability". Two sorts of chatbots are formulated, one with and one without personalisation factors. the planning of this research may be a two-by-two factorial design. The independent variables are the two chatbots (unpersonalised versus personalised) and thus the speci?c task or goal the user are ready to do with the chatbot within the ?nancial ?eld (a simple versus a posh task). The results are that there was no noteworthy interaction effect between personalisation and task on the user experience of chatbots. A signi?cant di?erence was found between the two tasks with regard to the user experience of chatbots, however this variation wasn't because of personalisation.
The Smart glasses Technology of wearable computing aims to identify the computing devices into today’s world.(SGT) are wearable Computer glasses that is used to add the information alongside or what the wearer sees. They are also able to change their optical properties at runtime.(SGT) is used to be one of the modern computing devices that amalgamate the humans and machines with the help of information and communication technology. Smart glasses is mainly made up of an optical head-mounted display or embedded wireless glasses with transparent heads- up display or augmented reality (AR) overlay in it. In recent years, it is been used in the medical and gaming applications, and also in the education sector. This report basically focuses on smart glasses, one of the categories of wearable computing which is very popular presently in the media and expected to be a big market in the next coming years. It Evaluate the differences from smart glasses to other smart devices. It introduces many possible different applications from the different companies for the different types of audience and gives an overview of the different smart glasses which are available presently and will be available after the next few years.
Future Applications of Smart Iot Devicesvivatechijri
With the Internet of Things (IoT) bit by bit creating as the resulting time of the headway of the Internet, it gets critical to see the diverse expected zones for the utilization of IoT and the research challenges that are connected with these applications going from splendid savvy urban areas, to medical care administrations, shrewd farming, collaborations and retail. IoT is needed to attack into for all expectations and purposes for all pieces of our day-to-day life. Despite the fact that the current IoT enabling advancements have immensely improved in the continuous years, there are so far different issues that require attention. Since the IoT ideas results from heterogeneous advancements, many examination difficulties will arise. In like manner, IoT is planning for new components of exploration to be finished. This paper presents the progressing headway of IoT advancements and inspects future applications.
Cross Platform Development Using Fluttervivatechijri
Today the development of cross-platform mobile application has under the state of compromise. The developers are not willing to choose an alternative of either building the similar app many times for many operating systems or to accept a lowest common denominator and optimal solution that will going to trade the native speed, accuracy for portability. The Flutter is an open-source SDK for creating high-performance, high fidelity mobile apps for the development of iOS and Android. Few significant features of flutter are - Just-in-time compilation (JIT), Ahead- of-time compilation (AOT compilation) into a native (system-dependent) machine code so that the resulting binary file can execute natively. The Flutter’s hot reload functionality helps us to understand quickly and easily experiment, build UIs, add features, and fix bugs. Hot reload works by injecting updated source code files into the running Dart Virtual Machine (VM). With the help of Flutter, we believe that we would be having a solution that gives us the best of both worlds: hardware accelerated graphics and UI, powered by native ARM code, targeting both popular mobile operating systems.
The Internet, today, has become an important part of our lives. The World Wide Web that was once a small and inaccessible data storage service is now large and valuable. Current activities partially or completely integrated into the physical world can be made to a higher standard. All activities related to our daily life are mapped and linked to another business in the digital world. The world has seen great strides in the Internet and in 3D stereoscopic displays. The time has come to unite the two to bring a new level of experience to the users. 3D Internet is a concept that is yet to be used and requires browsers to be equipped with in-depth visualization and artificial intelligence. When this material is included, the Internet concept of material may become a reality discussed in this paper. In this paper we have discussed the features, possible setting methods, applications, and advantages and disadvantages of using the Internet. With this paper we aim to provide a clear view of 3D Internet and the potential benefits associated with this obviously cost the amount of investment needed to be used.
Recommender System (RS) has emerged as a significant research interest that aims to assist users to seek out items online by providing suggestions that closely match their interests. Recommender system, an information filtering technology employed in many items is presented in internet sites as per the interest of users, and is implemented in applications like movies, music, venue, books, research articles, tourism and social media normally. Recommender systems research is usually supported comparisons of predictive accuracy: the higher the evaluation scores, the higher the recommender. One amongst the leading approaches was the utilization of advice systems to proactively recommend scholarly papers to individual researchers. In today's world, time has more value and therefore the researchers haven't any much time to spend on trying to find the proper articles in line with their research domain. Recommender Systems are designed to suggest users the things that best fit the user needs and preferences. Recommender systems typically produce an inventory of recommendations in one among two ways -through collaborative or content-based filtering. Additionally, both the general public and also the non-public used descriptive metadata are used. The scope of the advice is therefore limited to variety of documents which are either publicly available or which are granted copyright permits. Recommendation systems (RS) support users and developers of varied computer and software systems to beat information overload, perform information discovery tasks and approximate computation, among others.
The study LiFi (Light Fidelity) demonstrates about how can we use this technology as a medium of communication similar to Wifi . This is the latest technology proposed by Harold Haas in 2011. It explains about the process of transmitting data with the help of illumination of an Led bulb and about its speed intensity to transmit data. Basically in this paper, author will discuss about the technology and also explain that how we can replace from WiFi to LiFi . WiFi generally used for wireless coverage within the buildings while LiFi is capable for high intensity wireless data coverage in limited areas with no obstacles .This research paper represents introduction of the Lifi technology,performance,modulation and challenges. This research paper can be used as a reference and knowledge to develop some of LiFitechnology.
Social media platform and Our right to privacyvivatechijri
The advancement of Information Technology has hastened the ability to disseminate information across the globe. In particular, the recent trends in ‘Social Networking’ have led to a spark in personally sensitive information being published on the World Wide Web. While such socially active websites are creative tools for expressing one’s personality it also entails serious privacy concerns. Thus, Social Networking websites could be termed a double edged sword. It is important for the law to keep abreast of these developments in technology. The purpose of this paper is to demonstrate the limits of extending existing laws to battle privacy intrusions in the Internet especially in the context of social networking. It is suggested that privacy specific legislation is the most appropriate means of protecting online privacy. In doing so it is important to maintain a balance between the competing right of expression, the failure of which may hinder the reaping of benefits offered by Internet technology
THE USABILITY METRICS FOR USER EXPERIENCEvivatechijri
THE USABILITY METRICS FOR USER EXPERIENCE was innovatively created by Google engineers and it is ready for production in record time. The success of Google is to attributed the efficient search algorithm, and also to the underlying commodity hardware. As Google run number of application then Google’s goal became to build a vast storage network out of inexpensive commodity hardware. So Google create its own file system, named as THE USABILITY METRICS FOR USER EXPERIENCE that is GFS. THE USABILITY METRICS FOR USER EXPERIENCE is one of the largest file system in operation. Generally THE USABILITY METRICS FOR USER EXPERIENCE is a scalable distributed file system of large distributed data intensive apps. In the design phase of THE USABILITY METRICS FOR USER EXPERIENCE, in which the given stress includes component failures , files are huge and files are mutated by appending data. The entire file system is organized hierarchically in directories and identified by pathnames. The architecture comprises of multiple chunk servers, multiple clients and a single master. Files are divided into chunks, and that is the key design parameter. THE USABILITY METRICS FOR USER EXPERIENCE also uses leases and mutation order in their design to achieve atomicity and consistency. As of there fault tolerance, THE USABILITY METRICS FOR USER EXPERIENCE is highly available, replicas of chunk servers and master exists.
Google File System was innovatively created by Google engineers and it is ready for production in record time. The success of Google is to attributed the efficient search algorithm, and also to the underlying commodity hardware. As Google run number of application then Google’s goal became to build a vast storage network out of inexpensive commodity hardware. So Google create its own file system, named as Google File System that is GFS. Google File system is one of the largest file system in operation. Generally Google File System is a scalable distributed file system of large distributed data intensive apps. In the design phase of Google file system, in which the given stress includes component failures , files are huge and files are mutated by appending data. The entire file system is organized hierarchically in directories and identified by pathnames. The architecture comprises of multiple chunk servers, multiple clients and a single master. Files are divided into chunks, and that is the key design parameter. Google File System also uses leases and mutation order in their design to achieve atomicity and consistency. As of there fault tolerance, Google file system is highly available, replicas of chunk servers and master exists.
A Study of Tokenization of Real Estate Using Blockchain Technologyvivatechijri
Real estate is by far one of the most trusted investments that people have preferred, being a lucrative investment it provides a steady source of income in the form of lease and rents. Although there are numerous advantages, one of the key downsides of real estate investments is lack of liquidity. Thus, even though global real estate investments amount to about twice the size of investments in stock markets, the number of investors in the real estate market is significantly lower. Block chain technology has real potential in addressing the issues of liquidity and transparency, opening the market to even retail investors. Owing to the functionality and flexibility of creating Security Tokens, which are backed by real-world assets, real estate can be made liquid with the help of Special Purpose Vehicles. Tokens of ERC 777 standard, which represent fractional ownership of the real estate can be purchased by an investor and these tokens can also be listed on secondary exchanges. The robustness of Smart Contracts can enable the efficient transfer of tokens and seamless distribution of earnings amongst the investors. This work describes Ethereum blockchainbased solutions to make the existing Real Estate investment system much more efficient.
Natural Is The Best: Model-Agnostic Code Simplification for Pre-trained Large...YanKing2
Pre-trained Large Language Models (LLM) have achieved remarkable successes in several domains. However, code-oriented LLMs are often heavy in computational complexity, and quadratically with the length of the input code sequence. Toward simplifying the input program of an LLM, the state-of-the-art approach has the strategies to filter the input code tokens based on the attention scores given by the LLM. The decision to simplify the input program should not rely on the attention patterns of an LLM, as these patterns are influenced by both the model architecture and the pre-training dataset. Since the model and dataset are part of the solution domain, not the problem domain where the input program belongs, the outcome may differ when the model is trained on a different dataset. We propose SlimCode, a model-agnostic code simplification solution for LLMs that depends on the nature of input code tokens. As an empirical study on the LLMs including CodeBERT, CodeT5, and GPT-4 for two main tasks: code search and summarization. We reported that 1) the reduction ratio of code has a linear-like relation with the saving ratio on training time, 2) the impact of categorized tokens on code simplification can vary significantly, 3) the impact of categorized tokens on code simplification is task-specific but model-agnostic, and 4) the above findings hold for the paradigm–prompt engineering and interactive in-context learning and this study can save reduce the cost of invoking GPT-4 by 24%per API query. Importantly, SlimCode simplifies the input code with its greedy strategy and can obtain at most 133 times faster than the state-of-the-art technique with a significant improvement. This paper calls for a new direction on code-based, model-agnostic code simplification solutions to further empower LLMs.
Response & Safe AI at Summer School of AI at IIITHIIIT Hyderabad
Talk covering Guardrails , Jailbreak, What is an alignment problem? RLHF, EU AI Act, Machine & Graph unlearning, Bias, Inconsistency, Probing, Interpretability, Bias
Best Practices of Clothing Businesses in Talavera, Nueva Ecija, A Foundation ...IJAEMSJORNAL
This study primarily aimed to determine the best practices of clothing businesses to use it as a foundation of strategic business advancements. Moreover, the frequency with which the business's best practices are tracked, which best practices are the most targeted of the apparel firms to be retained, and how does best practices can be used as strategic business advancement. The respondents of the study is the owners of clothing businesses in Talavera, Nueva Ecija. Data were collected and analyzed using a quantitative approach and utilizing a descriptive research design. Unveiling best practices of clothing businesses as a foundation for strategic business advancement through statistical analysis: frequency and percentage, and weighted means analyzing the data in terms of identifying the most to the least important performance indicators of the businesses among all of the variables. Based on the survey conducted on clothing businesses in Talavera, Nueva Ecija, several best practices emerge across different areas of business operations. These practices are categorized into three main sections, section one being the Business Profile and Legal Requirements, followed by the tracking of indicators in terms of Product, Place, Promotion, and Price, and Key Performance Indicators (KPIs) covering finance, marketing, production, technical, and distribution aspects. The research study delved into identifying the core best practices of clothing businesses, serving as a strategic guide for their advancement. Through meticulous analysis, several key findings emerged. Firstly, prioritizing product factors, such as maintaining optimal stock levels and maximizing customer satisfaction, was deemed essential for driving sales and fostering loyalty. Additionally, selecting the right store location was crucial for visibility and accessibility, directly impacting footfall and sales. Vigilance towards competitors and demographic shifts was highlighted as essential for maintaining relevance. Understanding the relationship between marketing spend and customer acquisition proved pivotal for optimizing budgets and achieving a higher ROI. Strategic analysis of profit margins across clothing items emerged as crucial for maximizing profitability and revenue. Creating a positive customer experience, investing in employee training, and implementing effective inventory management practices were also identified as critical success factors. In essence, these findings underscored the holistic approach needed for sustainable growth in the clothing business, emphasizing the importance of product management, marketing strategies, customer experience, and operational efficiency.
A brand new catalog for the 2024 edition of IWISS. We have enriched our product range and have more innovations in electrician tools, plumbing tools, wire rope tools and banding tools. Let's explore together!
In May 2024, globally renowned natural diamond crafting company Shree Ramkrishna Exports Pvt. Ltd. (SRK) became the first company in the world to achieve GNFZ’s final net zero certification for existing buildings, for its two two flagship crafting facilities SRK House and SRK Empire. Initially targeting 2030 to reach net zero, SRK joined forces with the Global Network for Zero (GNFZ) to accelerate its target to 2024 — a trailblazing achievement toward emissions elimination.
Profiling of Cafe Business in Talavera, Nueva Ecija: A Basis for Development ...IJAEMSJORNAL
This study aimed to profile the coffee shops in Talavera, Nueva Ecija, to develop a standardized checklist for aspiring entrepreneurs. The researchers surveyed 10 coffee shop owners in the municipality of Talavera. Through surveys, the researchers delved into the Owner's Demographic, Business details, Financial Requirements, and other requirements needed to consider starting up a coffee shop. Furthermore, through accurate analysis, the data obtained from the coffee shop owners are arranged to derive key insights. By analyzing this data, the study identifies best practices associated with start-up coffee shops’ profitability in Talavera. These findings were translated into a standardized checklist outlining essential procedures including the lists of equipment needed, financial requirements, and the Traditional and Social Media Marketing techniques. This standardized checklist served as a valuable tool for aspiring and existing coffee shop owners in Talavera, streamlining operations, ensuring consistency, and contributing to business success.
How to Manage Internal Notes in Odoo 17 POSCeline George
In this slide, we'll explore how to leverage internal notes within Odoo 17 POS to enhance communication and streamline operations. Internal notes provide a platform for staff to exchange crucial information regarding orders, customers, or specific tasks, all while remaining invisible to the customer. This fosters improved collaboration and ensures everyone on the team is on the same page.
1. VIVA-Tech International Journal for Research and Innovation Volume 1, Issue 3 (2020)
ISSN(Online): 2581-7280 Article No. 4
PP 1-6
1
www.viva-technology.org/New/IJRI
STUDY OF MPS UNDER STRESSED CONDITIONS
Dr. Shwetali Kiran Churi1
1
(Department Of CHEMISTRY, MUMBAI University, MUMBAI-98, VIVA Institute of Technology, India)
Email id: skchuri@gmail.com
Abstract: This study is done to access the chemical stability of the candidate compound in the pharmaceuticals.
Usually, it is performed at the preliminary stage in the process of drug development. Forced degradation/ stress
testing is performed under accelerated environment. The experimental conditions cause the candidate compound
to degrade under extreme conditions like acid and base hydrolysis, peroxide oxidation, photo-oxidation and
thermal stability to identify the resultant degradation products. This helps to establish degradation pathways and
thus intrinsic stability of a drug substance. The stability of product describes shelf life and storage conditions and
helps in the selection of appropriate formulations and their suitable packaging. This is compulsory for regulatory
documentation. The commonly used analytical approach for FDS is HPLC with UV and/ or MS but these
techniques consume a lot of time and not provide high resolution to confirm the precise detection of degradation
products. Use of UPLC with photodiode array and MS analysis supports the identification of degradation
products and also reduces the time needed to evolve stability indicating methods.
Keywords – Pharmaceuticals , Degradation, Stability Hydrolysis, Oxidation.
1. INTRODUCTION
N1 - ( 3 - Methoxypyrazin - 2 - yl) sulphanilamide is a long acting sulfonamide that has been used in
the treatment of urinary tract infections and respiratory due to sensitive organisms by oral route of
administration.MPS is given with pyrimethamine in the treatment of malaria.[1,2]It has also been given in the
ratio 4 parts of N1 - ( 3 - Methoxypyrazin - 2 - yl) sulphanilamide to 5 parts of trimethoprim as a combination
with uses similar to those of co - trimoxazole 1.[3,4]
N
N
H
N
O
S
O
O
H2N
Molecular formula:C11H12N4O3S
Molecular Weight.: 280.3
N1
-(3-Methoxypyrazin-2-yl)sulphanilamide
Fig: 1 Chemical structures of solifenacin. [5]
Literature search reports few bio analytical methods for the quantitation of N1 - (3 - Methoxypyrazine -
2-yl) sulphanilamide (MPS) concentration in biological fluid samples using liquid chromatography and mass
spectroscopic method.[6,7] So far, the active pharmaceutical ingredient (API) to MPS as a published report
describing the complete characterization of impurities, are there.[8,9] MPS active pharmaceutical ingredient (API)
in the respective objects isolation / synthesis of LC / MS / MS are no reports on the use.
2. VIVA-Tech International Journal for Research and Innovation Volume 1, Issue 3 (2020)
ISSN(Online): 2581-7280 Article No. 4
PP 1-6
2
www.viva-technology.org/New/IJRI
Profiling of drug substance for its impurities is a critical parameter which determines the safety of the
drug substance as well as the controls required during manufacturing to ensure appropriate level of
impurities.[10,11] Identification and characterization of Impurities in pharmaceutical production, the acceptable
limit of 0.1 % of the present [10,12] is mandated. The present study details the identification and determination
of structure of few process related impurities found in the product (MPS). [13,14]Though, different methods of
synthesis of MPS are reported,[15,16] the selected route was safe, feasible & economical. However, these did not
give information regarding possible impurities. Impurity profiling of drugs in pharmaceutical analysis is an
important topic - the high purity of the drug substance manufacturing process technology to develop and deliver
safe drugs.[17,18,19]
2. EXPERIMENTAL
Preparation of solutions for under stressed conditions was used as given below:
a)Parent sample: Take accurate quantity of about 25.00 mg of MPS in a volumetric flask of 50 cm3
capacity
add 5.0 cm3
of diluent and sonicate to dissolve the sample and with the diluent make up the
volume.(Concentration : 500 ppm)
b)Acid Hydrolysis: Take accurate quantity of about 25.00 mg of MPS in a volumetric flask of 50 cm3
capacity.
Add 5.0 cm3
of 1N Hydrochloric acid, heat at 60 degree Celsius in water bath for 3 hours for Acid hydrolysis
and cool and then add 5.0 cm3
of 1 N NaOH for neutralization and with the diluent make up the volume.
(Diluent blank solution was also prepared in same manner without MPS and disregard peaks due to blank in the
test sample if any)
c)Base Hydrolysis: Take accurate quantity of about 25.00 mg of MPS in a volumetric flask of 50 cm3
capacity.
Add 5.0 cm3
of 1 N NaOH, heat at 60 degree Celsius in water bath for 3 hours for base hydrolysis and cool and
then add 5.0 cm3
of 1N Hydrochloric acid for neutralization and with the diluent make up the volume. (Diluent
blank solution was also prepared in same manner without MPS and disregard peaks due to blank in the test
sample, if any)
d)Aqueous (Humidity): Take accurate quantity of about 25.00 mg of MPS in a volumetric flask of 50 cm3
capacity. Add 5.0 cm3
of water, heat at 60 degree Celsius in water bath for 3 hours for aqueous hydrolysis and
cool and with the diluent make up the volume. (Diluent blank solution was also prepared in same manner
without MPS and disregard peaks due to blank in the test sample, if any)
e)Oxidation: Take accurate quantity of about 25.00 mg of MPS in a volumetric flask of 50 cm3
capacity. Add
5.0 cm3
of 5 % v/v hydrogen peroxide solution, heat at 60 degree Celsius in water bath for 3 hours for Oxidation
and cool and with the diluent make up the volume. (Diluent blank solution was also prepared in same manner
without MPS and disregard peaks due to blank in the test sample if any)
f)Photolytic Exposure: 1.00 g MPS was exposed in photolytic stability chamber. Solution was prepared as
same as parent sample.
g)Thermal Exposure: 1.00 g of MPS Batch No9025-P kept in oven at 105°C for 3.0 hrs and analyzed by
HPLC. Solution was prepared as same as parent compound.
..
Fig. 1 MPS crude sample chromatogram
3. VIVA-Tech International Journal for Research and Innovation Volume 1, Issue 3 (2020)
ISSN(Online): 2581-7280 Article No. 4
PP 1-6
3
www.viva-technology.org/New/IJRI
.
Fig. 2 Chromatogram of Acid hydrolysis of MPS under stressed condition
.
Fig. 3 Chromatogram of Base hydrolysis of MPS under stressed condition
Fig. 4 Chromatogram of Oxidation of MPS under stressed condition
4. VIVA-Tech International Journal for Research and Innovation Volume 1, Issue 3 (2020)
ISSN(Online): 2581-7280 Article No. 4
PP 1-6
4
www.viva-technology.org/New/IJRI
Fig. 5 Chromatogram of Aqueous (humidity) of MPS under stressed condition
Fig. 6 Chromatogram of Photolytic Exposure of MPS under stressed condition
Fig. 7 Chromatogram of Thermal Exposure of MPS under stressed condition.
3. RESULTS AND DISCUSSION
Peak Purity of the principle Peak chromatographic peaks under stressed condition gave the following
results:
1) Under the degradation condition, the parent sample showed five degradation impurities, 0.09% of total
impurities degradation, 99.91% of MPS and PDA analysis showed the homogeneity of peak (Purity angle
< Purity threshold).
5. VIVA-Tech International Journal for Research and Innovation Volume 1, Issue 3 (2020)
ISSN(Online): 2581-7280 Article No. 4
PP 1-6
5
www.viva-technology.org/New/IJRI
2) Under the degradation condition, the aqueous hydrolysis showed five degradation impurities, 0.14%
of total impurities degradation, 99.89% of MPS and PDA analysis showed the homogeneity of peak
(Purity angle < Purity threshold).
3) Under the degradation condition, the acid hydrolysis showed ten degradation impurities, 5.61% of
total impurities degradation, 94.40% of MPS and PDA analysis showed the homogeneity of peak (Purity
angle < Purity threshold).
4) Under the degradation condition, the base hydrolysis showed ten degradation impurities, 0.40% of
total impurities degradation, 99.60% of MPS and PDA analysis showed the homogeneity of peak (Purity
angle < Purity threshold).
5) Under the degradation condition, the oxidation showed forty six degradation impurities, 23.09% of
total impurities degradation, 76.91% of MPS and PDA analysis showed the homogeneity of peak (Purity
angle < Purity threshold).
6) Under the degradation condition, the thermal exposure showed five degradation impurities, 0.09% of
total impurities degradation, 99.9% of MPS and PDA analysis showed the homogeneity of peak (Purity
angle < Purity threshold).
7) Under the degradation condition, the photolytic exposure showed five degradation impurities, 0.13%
of total impurities degradation, 99.82% of MPS and PDA analysis showed the homogeneity of peak
(Purity angle < Purity threshold).
4. CONCLUSION
Peak purity of main peak in all conditions of force degradation passes. PDA Scan for degraded drug
substance and drug product is comparable to that of untreated drug substance and drug product. All peaks due to
degradation are well separated from each other and from main peak. So there is no interference of blank, placebo
and degradant at retention time of main peak observed in MPS drug.
This study relates that MPS-I, MPS-II, MPS, & MPS-III are well separated & comply with peak purity
parameter i.e. purity angle <purity threshold.
5. ACKNOWLEDGEMENT
The author is very thankful to Mrs. Minal A. Kudu and Merck, for providing facilities, equipments and
for providing samples.
REFERENCES
[1] Timothy McGovern, David Jacobson-Kram, (2006), “Regulation of genotoxic and carcinogenic impurities in drug substances and
products”, TrAC, Trends in Analytical Chemistry 25(8), 790-795.
[2] Colombo P., Betini R., Peracchia M.T., Santi P; (2000), Controlled Release Dosage Forms: From Ground to Space, European
Journal of Drug Metabolism and Pharmacokinetics, 21, 87-91.
[3] Indian Pharmacopoiea, (2010), Indian Pharmacopoeia commission, Ghaziabad, 6(1), 656-658.
[4] USP 32 – NF 27, General Chapter 1225, Validation of Compendial Methods, 2009.
[5] USP 32 – NF 27, General Chapter 1226, Verification of Compendial Methods, 2009.
[6] ICH Q3A(R) (2000), International Conferences on Harmonization, Draft Revised Guidance on Impurities in New Drug Substances.
Federal Register, 65(140), 45085-45090.
[7] ICH Q3B(R) (2000), International Conferences on Harmonization, Draft Revised Guidance on Impurities in New Drug Products.
Federal Register, 65(139), 44791- 44797.
[8] ICH Harmonized Tripartite Guideline, ICH Q2A, (1998), Text on Validation of Analytical procedures.
[9] CITAC/EURACHEM, (2002), Working Group, International guide to quality in analytical chemistry: An aid to accreditation.
6. VIVA-Tech International Journal for Research and Innovation Volume 1, Issue 3 (2020)
ISSN(Online): 2581-7280 Article No. 4
PP 1-6
6
www.viva-technology.org/New/IJRI
[10] ICH Harmonized Tripartite Guideline, ICH Q2B, (1997), Validation of Analytical procedures: Methodology.
[11] Reviewer Guidance: Validation of chromatographic Methods, Centre for Drug and Research, (2004), U.S. Government Printing
office, Washington DC.
[12] U.S. FDA, Title 21 of the U.S. Code of Federal Regulations: 21 CFR 211—Current good manufacturing practice for finished
pharmaceuticals.
[13] U.S. FDA - Guidance for Industry (draft) Analytical Procedures and Methods (2000), Validation: Chemistry, Manufacturing, and
Controls and Documentation.
[14] ISO/IEC 17025, (2005), General requirements for the competence of testing and calibration laboratories.
[15] International Conference on Harmonization (ICH) of Technical Requirements for the Registration of Pharmaceuticals for Human
Use, Validation of analytical procedures: definitions and terminology, (2000), Geneva.
[16] International Conference on Harmonization (ICH) of Technical Requirements for the Registration of Pharmaceuticals for Human
Use, Validation of analytical procedures: Methodology, adopted in (2000), Geneva.
[17] U.S. EPA, Guidance for methods development and methods validation for the Resource Conservation and Recovery Act (RCRA)
Program, Washington, D.C., (1995)., http://www.epa.gov/sw-846/pdfs/methdev.pdf. Last Accessed on 17 July 2018.
[18] General Chapter 1225, (2007), Validation of compendial methods, United States Pharmacopeia 30, National Formulary 25,
Rockville, Md., USA, The United States Pharmacopeial Convention, Inc
[19] U.S. FDA - Guidance for Industry, Bioanalytical Method Validation.