International Journal of Research In Pharmaceutical Chemistry and Analysis
Rubatosis Publication has launched its scientific journal named International Journal of Research in Pharmaceutical Chemistry and Analysis (IJRPCA ISSN (Online): 2582-1970) IJRPCA will be published quarterly per year in January, April, July, and October. The journal publishes original research work that contributes significantly to further the scientific knowledge in Pharmaceutical Chemistry and Analysis.
Stability indicating RP-HPLC method for the estimation of flucloxacillin sodium in a tablet dosage form
A Simple, accurate and precise method was developed and validated for the determination of flucloxacillin sodium in its tablet dosage form. The separation was eluted on xterra c18 column (4.6x150mm, 5micron) using a mixture of octane buffer and methanol as mobile phase in a ratio of (30:70) which was pumped through column at a flow rate of 1ml/min. Optimised wavelength for flucloxacillin was 237nm, the retention time was 2.305minutes and the percentage purity was found to be 98.14%. System suitability parameters such as theoretical plate and tailing factor for flucloxacillin sodium was found to be 2991.64 and 1.90 respectively, the proposed method was validated as per ICH guidelines (ICH, Q2 AND (R1)) the method was found to be linear at the concentration range of 20-100µg/ml and the correlation coefficient (r2) value was found to be 0.9994 percentage RSD for precision was 0.9% and percentage RSD for ruggedness was 0.5%. The precision study was precise, robust and repeatable. The LOD and LOQ values are 2.98 and 9.98 respectively. Hence the suggested RP-HPLC method can be used for routine analysis for flucloxacillin sodium in tablet dosage form.
Copyright (c) 2020 https://creativecommons.org/licenses/by-nc-nd/4.0
A robust stability indicating HPLC technique for evalution of Pibrentasvir and Glecaprevir in tablet dosage form
When liver cells gets infected and vandalized, the condition is termed as Hepatitis. HCV therapy is performed with mixture of drugs. For the combined evaluation of Pibrentasvir and Glecaprevir in tablets, a rapid, selective and robust HPLC technique stability indicating was developed herein this work. Analysis was executed by Cosmicsil, with dimensions 250 mm by 4.6 mm column and mobile phase possessing KH2PO4 with 0.1M, 65 ml and 35 ml of methanol and 230 nm of PDA analysis. Elution times were found out as were 1.663 min and 2.249 min, for Pibrentasvir and Glecaprevir respectively with linear ranges 20µg/ml, 60 µg/ml and 50 µg/ml, 150 µg/ml, respectively having detection limits as 0.190 µg/ml and 0.207 µg/ml and quantization limits as 0.634 µg/ml and 0.690 µg/ml. This method is explicit having RSD values as 0.097% Pibrentasir & 0.232% Glecaprevir showing an accuracy of between 98.82 and 100.07% for Pibrentasir 99.31, Glecaprevir 100.45% recovery values. During the investigation of degradation, peaks elution times of degradants greatly varied with the elution times of Glecaprevir and Pibrentasvir thus, proving method‘s power of stability indication and specificity. The validation and degradation stability studies were carried out according to ICH and ICH Q1B Guidelines.
A Photo Stability Indicating HPLC technique for Validation of Netupitant and Palonosetron in Bulk and Formulations
Analytical chemistry is the science that seeks ever improved means of measuring the chemical composition of natural and artificial materials.Netupitant Delayed emesis has been largely associated with the activation of tachykinin family neurokinin 1 receptors. Palonosetron is a selective serotonin 5-HT3 receptor antagonist. The antiemetic activity of the drug is brought about through the inhibition of 5-HT3 receptors present both centrally and peripherally in turn inhibits the visceral afferent stimulation of the vomiting center.The mobile phase used was orthophosphoric and acetate 70% buffer pH 3 and 30% methanol.The assay of Netupitant and Palanosetron was performed with tablets and the % assay was found to be 100.08 and 100.04, The linearity was found to be linear with a correlation coefficient of 0.999, the precision 0.8 and 0.3 for Netupitant and Palanosetron which shows that the method is precise.The validation of developed method shows that the accuracy is well within the limit, which shows that the method is capable of showing good accuracy and reproducibility. The LOD and LOQ for Netupitant were found to be 3.02 and 9.98 and LOD and LOQ for Palanosetron was found to be 3.00 and 10.00. Thus, it shows that the method is stability indicating, sensitive, accurate, robust and precise. Hence, the developed HPLC method can be successfully applied to the pharmaceutical dosage form and can be used for routine analysis.
Development and validation of UV-visible spectrophotometric method for determination of Bicalutamide in bulk and in pharmaceutical dosage form
The aim of the present study, simple and sensitive spectrophotometric method was developed for the estimation and validation of Bicalutamide in bulk and Pharmaceutical dosage form by UV spectroscopy as per ICH guidlines. The maximum absorbance (λmax) of Bicalutamide in methanol was found to be 272 nm against methanol as a blank. The Bicalutamide obeys the Beers law in the concentration range 2.5 to 15 μg/ml with a correlation coefficient of 0.999. The proposed method was applied for the estimation of Bicalutamide in pharmaceutical dosage form and % purity was found to be 99.96 to 100.06 that indicate the good agreement with the label claim. The accuracy of the proposed method was determined by recovery study at three different levels (50%, 100%, and 150%). The % recovery was found to be 99.6 to 100.2%. The precision study was carried out by intraday and interday. The % RSD was found to be < 2 which indicates that the method is precise. The proposed method was a fast technique for the routine analysis of Bicalutamide in bulk and pharmaceutical dosage form.
Copyright (c) 2021 https://creativecommons.org/licenses/by-nc-nd/4.0
Validation of high performance liquid chromatography mass spectrometric method in negative ion mode for the estimation of Amlopdipine in human plasma using Amlopdipine D3 as internal standard
Pharmaceutical analysis plays a very prominent role in quality assurance as well as quality control of bulk drugs and pharmaceutical formulations. Rapid increase in pharmaceutical industries and production of drug in various parts of the world has brought a rise in demand for new analytical techniques in the pharmaceutical industries. As a consequence, analytical method development has become the basic activity of analysis. Recent development in analytical methods has been resulted from the advancement of analytical instruments. The improvement of the analytical method development and analytical instruments have reduced the time of analysis, increased precision and accuracy and reduced costs of analysis. As a consequence, most of pharmaceutical organizations are investing huge amount of money for the establishment of advanced analytical laboratories. Analytical techniques are developed and validated for active pharmaceutical ingredients (API), excipients, drug products, degradation products and related substances, residual solvents, etc. As a result, it has become an integral part of the requirements of the regulatory organization. Analytical method development finally results in official test methods. These methods are used in quality control laboratories to ensure the identity, purity, safety, efficacy and performance of drug products. Regulatory authorities are placing greater emphasis on analytical methods in manufacturing. Drug approval by regulatory authorities requires the applicant to prove control of the entire process of drug development by using validated analytical methods.
Validation of high performance liquid chromatography mass spectrometric method in positive ion mode for the estimation of Clopidogrel in human plasma using Clopidogrel D4 as internal standard
The present project work was to develop a robust, rapid, simple and sensitive liquid chromatography mass spectrometry (LC-MS/MS) assay method for the quantification of clopidogrel in human plasma. A high performance liquid chromatography mass spectrometric method for the estimation of clopidogrel, in human plasma in positive ion mode was developed and validated using clopidogrel d4 as internal standard (is). Sample preparation was accomplished by solid phase extraction method. The eluted samples were chromatographed on kromasil 100 5c18, 100 x 4.6 mm, 5 µm (make: akzo nobel) using a mobile phase consisting of hplc grade acetonitrile: milli q/hplc grade water (90:10, v/v) the method was validated over a concentration range of 0.031 ng/ml to 15.077 ng/ml for clopidogrel. This validation report provides the results of analyte selectivity, matrix selectivity, matrix effect, sensitivity determinations, calibration standards and quality control samples data, precision and accuracy data, the results of recovery, various stabilities, run size evaluation and dilution integrity along with all pertinent documentation.
Validation of high performance liquid chromatography mass spectrometric method in negative ion mode for the estimation of Monomethyl fumarate in human plasma using Monomethyi fumarate D3 as internal standard
The present project work was to develop a robust, rapid, simple and sensitive liquid chromatography mass spectrometry (LC-MS/MS) assay method for the quantification of monomethyl fumarate in human plasma. An analytical method employing LC-MS/MS using human plasma was developed and fully validated for the estimation of Monomethyl fumarate in human plasma by using monomethyl fumarateD3 as internal standarad. The solid phase extraction technique (SPE) was used for the extraction of the drug and Internal standard (IS). The chromatographic separation was achieved on a Zodiac C18 column by using a 70:30 (v/v) mixture of acetonitrile and 0.1% formic acid as the mobile phase at a flow rate of 0.5 mL/min. Totally five precision and accuracy batches were performed during the entire validation and intra-day and inter-day precision and accuracy were proved. KEYWORDS: Monomethyl fumarate, Human plasma, LC–MS/MS, Pharmacokinetics, Quantification.
Analytical method development and validation of Rasagiline mesylate in bulk and doasage form by UV spectroscopy
A simple, rapid and precise uv spectroscopy method was developed for quantitative determination of rasagiline mesylate in bulk and dosage forms. This method was based on the beer’s lamberts law and The linearity was found to be in the concentration range of 50-300µg/ml and maximum absorbance was measured at 263nm 0.1m sulphuric acid as a solvent. The method was validated statistically and by recovery studies. Recovery was found to be in the range of 98 -102% and the %R.S.D was found to be less than 2%. The proposed method was economical and sensitive for the estimation of Rasagiline Mesylate (RM) in bulk and tablet dosage.
A new analytical method for determination of ledipasvir and sofosbuvir in pharmaceutical formulations by HPLC method
A simple, Accurate, precise method was developed for the simultaneous estimation of the Sofosbuvir and Ledipasvir in Tablet dosage form. Chromatogram was run through Std Discovery C8 150 x 4.6 mm, 5m. Mobile phase containing Buffer 0.1% OPA: Acetonitrile taken in the ratio 60:40 was pumped through column at a flow rate of 1 ml/min. Buffer used in this method was 0.1% OPA buffer. Temperature was maintained at 30°C. Optimized wavelength selected was 260 nm. Retention time of Sofosbuvir and Ledipasvir were found to be 2.367 min and 3.436 min. %RSD of the Sofosbuvir and Ledipasvir were and found to be 0.6 and 0.5 respectively. %Recovery was obtained as 99.61% and 99.80% for Sofosbuvir and Ledipasvir respectively. LOD, LOQ values obtained from regression equations of Sofosbuvir and Ledipasvir were 0.67, 2.02 and 0.70, 2.12 respectively. Regression equation of Sofosbuvir is y = 4266.x + 7700, and y = 4861.x + 2656.of Ledipasvir. Retention times were decreased and run time was decreased, so the method developed was simple and economical that can be adopted in regular Quality control test in Industries.
Copyright (c) 2019 https://creativecommons.org/licenses/by-nc-nd/4.0
A new analytical method for determination of dolutegravir and rilpivirine in pharmaceutical formulations by RP-HPLC method
A simple, rapid, precise, sensitive and reproducible reverse phase high performance liquid chromatography (RP-HPLC) method has been developed for the quantitative analysis of Dolutegravir and Rilpivirine in pharmaceutical dosage form. Chromatographic separation of Dolutegravir and Rilpivirine was achieved on Waters Alliance -2695, by using Luna C18 (250mm x 4.6mm, 5µm) column and the mobile phase containing 0.1% OPA & ACN in the ratio of 50:50 v/v. The flow rate was 1.0 ml/min, detection was carried out by absorption at 245 nm using a photodiode array detector at ambient temperature. The number of theoretical plates and tailing factor for Dolutegravir and Rilpivirine were NLT 2000 and should not more than 2 respectively. The linearity of the method was excellent over the concentration range 10-150 µg/ml and 5-75 µg/ml for Dolutegravir and Rilpivirine respectively. The correlation coefficient was 0.999. % Relative standard deviation of peak areas of all measurements always less than 2.0. The proposed method was validated according to ICH guidelines. The method was found to be simple, economical, suitable, precise, accurate & robust method for quantitative analysis of Dolutegravir and Rilpivirine study of its stability.
A new analytical method for determination of tenofovir disoproxil fumarate and emtricitabine in pharmaceutical formulations by RP-HPLC method
A simple, rapid, precise, sensitive and reproducible reverse phase high performance liquid chromatography (RP-HPLC) method has been developed for the quantitative analysis of Tenofovir Disoproxil Fumarate and Emtricitabine in pharmaceutical dosage form. Chromatographic separation of Tenofovir Disoproxil Fumarate and Emtricitabine was achieved on Waters Alliance -2695, by using Luna C18 (250mm x 4.6mm, 5µm) column and the mobile phase containing 0.1% TEA adjusted pH-2.5 with OPA & ACN in the ratio of 60:40 v/v. The flow rate was 1.0 ml/min, detection was carried out by absorption at 261 nm using a photodiode array detector at ambient temperature. The number of theoretical plates and tailing factor for Tenofovir Disoproxil Fumarate and Emtricitabine were NLT 2000 and should not more than 2 respectively. The linearity of the method was excellent over the concentration range 30-450 µg/ml and 20-300 µg/ml for Tenofovir Disoproxil Fumarate and Emtricitabine respectively. The correlation coefficient was 0.999. % Relative standard deviation of peak areas of all measurements always less than 2.0. The proposed method was validated according to ICH guidelines. The method was found to be simple, economical, suitable, precise, accurate & robust method for quantitative analysis of Tenofovir Disoproxil Fumarate and Emtricitabine study of its stability.
Method developed for the determination of apixaban by using U.V. spectrophotometric
The present work is aim to Develop UV spectrophotometry method for the estimation of Apixaban in its dosage forms. Analysed the marketed formulations for their reliability and accuracy and Performed the recovery studies for the developed UV spectrophotometric method. The developed method was validate for its accuracy precision reproducibility. On the basis of results the UV spectrophotometric method developed for the determination of Apixaban is found to be precise, accurate and cost effective. Hence this method can be used for routine analysis of Apixaban in bulk and pharmaceutical dosage forms.
Development and validation of new analytical method for the estimation of fluoxetine in bulk and dosage form by UV spectrophotometry
A simple, rapid and precise method is developed for the quantitative determination of Fluoxetine in combined pharmaceutical-dosage forms. The method was based on UV Spectrophotometric determination of Fluoxetine drug using Beer-Lamberts Law. It involves absorbance measurement at 224 nm (λmax of Fluoxetine) in water. For UV Spectrophotometric method, linearity was obtained in concentration range of 5-30 mcg/ml with regression 0.999 for Fluoxetine respectively. Recovery was in the range of 98 -102%; the value of standard deviation and %R.S.D was found to be < 2 shows high precision of the method..
Stability indicating RP-HPLC method development and validation for the simultaneous estimation of ceftriaxone and tazobactum in sterile powder for injection
A simple, rapid, precise and accurate method is developed for the quantitative simultaneous determination of ceftriaxone and tazobactum in bulk and pharmaceutical formulations. Separation of ceftriaxone and tazobactum was successfully achieved by using Inertsil C18 ODS column 250X4.6mm, 5µm in an isocratic mode using water and acetonitrile (80:20) at a flow rate of 1.0 ml/min and was monitored at 254 nm with a retention time of 3.049 minutes and 4.317 minutes for ceftriaxone and tazobactum respectively. The method was validated and the response was found to be linear in the drug concentration range of 20µg/ml to 80 µg/ml for ceftriaxone and 5 µg/ml to 35 µg/ml for tazobactum. The values of the correlation coefficient were found to be 0.999 for ceftriaxone and 0.999 for tazobactum respectively. The LOD and LOQ for ceftriaxone were found to be 0.021 and 0.064 respectively. The LOD and LOQ for tazobactum were found to be 0.030 and 0.091 respectively. The percentage recovery for ceftriaxone and tazobactum were found to be 98-102% respectively which indicates that the proposed method is highly accurate. The specificity of the method shows good correlation between retention times of standard with the sample. The method was extensively validated according to ICH guidelines for Linearity, Accuracy, Precision, Specificity and Robustness. Stability of the drugs was determined by using acid/base, thermal, oxidative stress testing.
Development and validation of new analytical method for the simultaneous estimation of omeprazole and domperidone in pharmaceutical dosage form by UV spectrophotometry
A simple, rapid and precise method was developed for the quantitative simultaneous determination of Omeprazole and Domperidone in combined pharmaceutical-dosage forms. The method was based on UV-Spectrophotometric determination of two drugs, using simultaneous equation method. It involves absorbance measurement at 291 nm (λmax of Omeprazole) and 289 nm (λmax of Domperidone) in Methanol: Acetonitrile (30:70 v/v). For UV Spectrophotometric method, linearity was obtained in concentration range of 1-15 µg/ml for Domperidone and 1-50 µg/ml for Omeprazole respectively, with regression 0.999 and 0.999 for Domperidone and Omeprazole respectively. Recovery was in the range of 99 -103%; the value of standard deviation and %R.S.D were found to be < 2 %; shows the high precision of the method., in accordance with ICH guidelines. The method has been successively applied to pharmaceutical formulation and was validated according to ICH guidelines.
Spectrophotometric determination and estimation of minoxidil in tablet dosage form by UV
A simple, precise, accurate and economical UV spectrophotometric method has been developed and validated for the estimation of Minoxidil in the tablet dosage form. Minoxidil shows maximum absorbance at 279.4nm. The method was carried out by using 0.1N HCl as a solvent. The drug shows linearity from the concentration range of 1-6µg/ml and correlation coefficient was found to be 0.9992. The proposed method was statistically validated for precision, accuracy, ruggedness, robustness, the limit of detection, quantitation as per the ICH guidelines. Hence this method can be successfully applied for routine analysis of Minoxidil in bulk and tablet dosage form.
Stability indicating method development and validation for the determination of haloperidol and benzhexol by RP-HPLC
A simple, Accurate, precise method was developed for the simultaneous estimation of the Haloperidol and Benzhexol in Tablet dosage form. The chromatogram was run through Kromasil (250mm 4.6mm, 5µ). Mobile phase containing Buffer and Acetonitrile and methanol in the ratio of 48:52 was pumped through column at a flow rate of 1.0 ml/min. The temperature was maintained at 30°C. The optimized wavelength for Haloperidol and Benzhexol was 220nm. The retention time of Haloperidol and Benzhexol were found to be 2.415 min and 2.820min. %RSD of the Haloperidol and Benzhexol were and found to be 0.6 and 0.2 respectively. %Recover was Obtained as 98.92% and 99.60% for Haloperidol and Benzhexol. LOD, LOQ values were obtained from regression equations of Haloperidol and Benzhexol were 0.42ppm, 1.27ppm and 0.04ppm, 0.14ppm respectively. Regression equation of Haloperidol is y = 24009x + 38704, and of Benzhexol is y = 40558x + 2880. Retention times are decreased and that run time was decreased so the method developed was simple and economical that can be adopted in regular Quality control test in Industries
Stability indicating RP-HPLC method development and validation for the simultaneous estimation of Grazoprevir and Elbasvir in bulk and pharmaceutical dosage form
A simple, Accurate and precise method was developed for the simultaneous estimation of the Grazoprevir and Elbasvir in Tablet dosage form. Chromatogram was run through Kromosil C18 (250 x 4.6 mm), 5m. Mobile phase containing Buffer: Acetonitrile taken in the ratio 45:55 was pumped through column at a flow rate of 1 ml/min. Buffer used in this method was Di Potassium Hydrogen ortho Phosphate. Temperature was maintained at 30°C. Optimized wavelength selected was 215 nm. Retention time of Elbasvir and Grazoprevir and were found to be 2.503 min and 3.004. %RSD of the Elbasvir and Grazoprevir were and found to be 0.3 and 0.4 respectively. %Recovery was obtained as 98.17% and 99.83% for Grazoprevir and Elbasvir respectively. LOD, LOQ values obtained from regression equations of Grazoprevir and Elbasvir were 0.24, 0.73 and 0.06, 0.19 respectively. Retention times were decreased and run time was decreased, so the method developed was simple and economical that can be adopted in regular Quality control test in Industries.
Copyright (c) 2018 https://creativecommons.org/licenses/by-nc-nd/4.0
RP-HPLC method development and validation for the estimation of antifungal drug terbinafine HCL in bulk and pharmaceutical dosage form
In the present work RP-HPLC method has been developed for the quantitative estimation of Terbinafine hydrochloride in bulk drug and pharmaceutical formulations. A rapid and sensitive RP-HPLC Method with PDA detection (220 nm) for routine analysis of in Bulk drug and Pharmaceutical formulation was developed. Chromatography was performed with mobile phase containing a mixture of Potassium dihydrogen phosphate and Acetonitrile (65:35 v/v) with flow rate 1.5 ml/min. The linearity was found to be in the range of 50-150 µg/ml with (r2=0.999). The proposed method was validated by determining sensitivity, accuracy, precision, LOD, LOQ and system suitability parameters according to ICH guidrelines.
Copyright (c) 2018 Rubatosis Publications https://creativecommons.org/licenses/by-nc/4.0
Development and validation of new analytical method for the simultaneous estimation of ibuprofen and diphenhydramine in bulk and pharmaceutical dosage form by RP-HPLC
A simple, accurate, rapid and precise method was developed for the simultaneous estimation of Ibuprofen and Diphenhydramine in Pharmaceutical dosage form. Chromatogram was run through Inertsil ODS (250x4.6mm) 5µ. Mobile phase used was Acetonitrile and Phosphate buffer (45:55) at a flow rate of 1.0 ml/min and detection wavelength was found to be 260 nm. The retention time was found to be 2.32 min and 2.93 min for Ibuprofen and Diphenhydramine respectively. The accuracy and reliability of the method was assessed by evaluation of linearity, precision (intra-day and inter-day % RSD >2), accuracy (98-102%), specificity, LOD, LOQ values in accordance with ICH guidelines. The developed method is applicable for routine quality control analysis of selected combined dosage forms.
Method development and method validation of guaifenesin and dextromethorphan by RP-HPLC
A new, simple, precise, accurate and reproducible RP-HPLC method for Simultaneous estimation of bulk and pharmaceutical formulations. Separation of Guaifenesin and Dextromethorphan was successfully achieve THERMO, C18, 250X4.6mm, 5µm or equivalent in an isocratic mode utilizing 0.1M KH2PO4: Methanol (60:40) at a flow rate of 1.0ml/min and eluate was monitored at 280nm, with a retention time of 3.259 and 4.164 minutes for Guaifenesin and Dextromethorphan respectively. The method was validated and there response was found to be linear in the drug concentration range of 50µg/ml to150 µg/ml for Guaifenesin and 50µg/ml to150 µg/ml for Dextromethorphan. The values of the correlation coefficient were found to 0.999 for Guaifenesin and 1for Dextromethorphan. respectively. The LOD and LOQ for Guaifenesin were found to be 0.597 and 1.991 respectively. The LOD and LOQ for Dextromethorphan were found to be 0.1072 and 0.3572 respectively. This method was found to be good percentage recovery for were found to be 99 and 100 respectively indicates that the proposed method is highly accurate. The specificity of the method shows good correlation between retention times of standard with the sample so, the method specifically determines the analyte in the sample without interference from excipients of tablet dosage forms. The method was extensively validated according to ICH guidelines for Linearity, Accuracy, Precision, Specificity and Robustness.
Synthesis, Characterize and Evaluation of anti-bacterial and anti-fungal activity of thiazines
1,3 – Thiazines have been applied as useful starting materials in the stereo selective synthesis of compounds of pharmacological interest and they have served as chiral ligants and auxiliaries in enantioselective transformation. The thiazines are of great importance because they act as precursor for the synthesis of Cephalosporins (3,6-dihydro-2H-,1,3-thiazine) and then converted to the thiazine derivatives (an heterocyclic compounds). Therefore, it was thought to combine chalcones moiety to thiazine derivative together in a molecular frame work to see the biological activities, additive effort of these rings towards biological activities like Anti- bacterial and Anti- fungal activities.