scholarly journals Novel stability-indicating RP-UPLC method for simultaneous estimation of sitagliptin and ertugliflozin in bulk and pharmaceutical formulations

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Ramya kuber B ◽  
Swetha Addanki
Keyword(s):  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Simultaneous Estimation ◽  
Uv Detector ◽  
Routine Examination ◽  
Limit Of Quantification ◽  
Stability Indicating ◽  
Ich Guidelines ◽  
Water Ph ◽  
By Products

Abstract Background The present investigation was proposed to develop a simple, sensitive, rapid, accurate, precise stability-indicating RP-UPLC method for simultaneous estimation of sitagliptin and ertugliflozin. Chromatographic separation was performed with Waters Hibar C8 [100×2.1mm, 2μ] column and mobile phase acetonitrile: water (pH 3.5) [50:50%, v/v], pumped at a flow rate 0.2ml/min. The separated analytes were detected with a UV detector at a wavelength of 218nm. Results The separation of sitagliptin and ertugliflozin was done at a retention time of 0.859min and 1.570min, respectively. The present method was validated according to the ICH guidelines Q2 R1, and stability-indicating studies were carried out as per ICH guidelines Q1A R2. Intra-day and inter-day precision were found to be within acceptable limits. The linearity of the proposed method was in the concentration range of 25–125μg/ml and 3.75–22.5μg/ml for sitagliptin and ertugliflozin, respectively. Limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.5μg/ml and 1.53μg/ml for sitagliptin and 0.13μg/ml and 0.38μg/ml for ertugliflozin, respectively. The recovery of the method was found in between 99.7% and 100.7%. Conclusion The proposed method was able to distinguish the analytes from by-products. Hence, the method was successfully implied for stability-indicating studies and for routine examination of sitagliptin and ertugliflozin in pharmaceutical formulation.

scholarly journals Stability indicating RP-UPLC method for simultaneous quantification of bempedoic acid and ezetimibe in bulk and pharmaceutical formulations

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Uma Sai Teja Yarra ◽  
Sowjanya Gummadi
Keyword(s):  
Present Method ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Simultaneous Estimation ◽  
Stability Studies ◽  
Uv Detector ◽  
Limit Of Quantification ◽  
Stability Indicating ◽  
Simultaneous Quantification ◽  
Ich Guidelines

Abstract Background Bempedoic acid and Ezetimibe acid are used in combination for treatment of hypercholesterolemia. The current work was undertaken to develop a simple and rapid stability-indicating RP-UPLC method for the simultaneous estimation of Bempedoic acid and Ezetimibe in tablets as no such method was available. The chromatographic separation was performed with Waters Acquity C18 [50 × 2.1 mm, 1.7 μ] column using methanol: acetonitrile: water [50: 30: 20, by volume] as mobile phase pumped at a flow rate 0.5 mL/min. The separated analytes were detected at 260 nm using UV detector. Results The separation of Bempedoic acid (BA) and Ezetimibe (EZ) was done at a retention time of 1.827 min. and 3.577 min. respectively. The validation and stability studies of the present method were carried out according to the ICH guidelines. The linearity of the proposed method was in the range of 30–130 μg/mL and 5–50 μg/mL for Bempedoic acid and Ezetimibe respectively. Limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.1216 μg/mL and 0.3685 μg/mL for Bempedoic acid and 0.1189 μg/mL and 0.3602 μg/mL for Ezetimibe respectively. The recovery of the method was found to be in the range of 99.89—100.31% for Bempedoic acid and 98.14—99.94% for Ezetimibe while the % RSD for both drugs in the precision and robustness study was less than 2.0. The drugs did not show any major degradants in the exposed conditions. Conclusion The developed method was found to be simple, sensitive, accurate, precise, robust, rapid and yet stability indicating. The method can be adopted for simultaneous estimation of Bempedoic acid and Ezetimibe in the pharmaceutical formulation.

scholarly journals Simultaneous Estimation and Validation of Atorvastatin Calcium and Aspirin in Combined Capsule Dosage Form by RP HPLC Method

2012 ◽  
Vol 9 (3) ◽  
pp. 1449-1456
Author(s):  
B. V. Suma ◽  
K. Kannan ◽  
V. Madhavan ◽  
Chandini R. Nayar
Keyword(s):  
Limit Of Detection ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Uv Detector ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Atorvastatin Calcium ◽  
Ich Guidelines ◽  
Phase Liquid ◽  
Liquid Chromatography Method

A new simple, specific, precise and accurate revere phase liquid chromatography method has been developed for estimation of atorvastatin calcium (AST) and ASPIRIN (ASP) simultaneously in a combined capsule dosage forms. The chromatographic separation was achieved on a 5 – micron C 18 column (250x 4.6mm) using a mobile phase consisting of a mixture of Acetonitrile: Ammonium Acetate buffer 0.02M (68:32) pH 4.5. The flow rate was maintained at 0.8 ml/min. The detection of the constituents was done using UV detector at 245 nm for AST and ASP. The retention time of AST and ASP were found be 4.5915 ± 0.0031 min and 3.282 ±0.0024 min respectively. The developed method was validated for accuracy, linearity, precision, limit of detection (LOD) and limit of quantification (LOQ) and robustness as per the ICH guidelines.

Development and Validation of the Analytical method for the estimation of a combination of 5-fluorouracil and Imiquimod by RP-HPLC

2021 ◽  
pp. 3313-3318
Author(s):  
Bhupender Tomar ◽  
Ankita Sharma ◽  
Inder Kumar ◽  
Sandeep Jain ◽  
Pallavi Ahirrao
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Simultaneous Estimation ◽  
Limit Of Quantification ◽  
Pharmaceutical Ingredients ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Development And Validation ◽  
Liquid Chromatographic

A simple, precise, and accurate reverse phase high performance liquid chromatographic method (RP-HPLC) was developed and validated for the estimation of the combination of 5- Fluorouracil (5-FU) and Imiquimod in active pharmaceutical ingredients (APIs). The method was carried out on Phenomenex C18 (250 × 4.6mm I.D., 5𝜇m) using isocratic elution mode. The mobile phase was used as Acetonitrile: 10mM potassium dihydrogen orthophosphate: triethylamine (40:59.9:0.1, v/v, pH 4.5 with orthophosphoric acid) and Water: ACN (50:50 v/v) was used as a diluent. The concentration of solvents was 1-20µg/ml and the volume of injection was 20µl with the flow rate of 1.2ml/min. The retention times for 5-FU and Imiquimod were found to be 1.9±0.5 and 6.6±0.5 min respectively. The absorption maxima of 5FU and Imiquimod were found 267nm and 227nm respectively. The method was validated as per ICH guidelines. All the data were found within the specified limits. The limit of detection (LOD) and limit of quantification (LOQ) of 5- Fluorouracil were found to be 0.015μg/mL and 0.048 μg/mL, respectively, and Imiquimod was found to be 0.078μg/mL and 0.237μg/mL, respectively. The method developed in the present study was found to be sensitive, specific, and precise and can be applied for the simultaneous estimation of 5-FU and Imiquimod.

A NOVEL STABILITY INDICATING RP-HPLC METHOD DEVELOPMENT AND VALIDATION FOR THE DETERMINATION OF VALSARTAN AND HYDROCHLOROTHIAZIDE IN BULK AND PHARMACEUTICAL FORMULATIONS

INDIAN DRUGS ◽  
2017 ◽  
Vol 54 (08) ◽  
pp. 54-61
Author(s):  
B. Venkateswara Rao ◽  
◽  
S. Vidyadhara ◽  
V. Basaveswara Rao
Keyword(s):  
Method Development ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Uv Detector ◽  
Chromatography Method ◽  
Stability Indicating ◽  
Liquid Chromatography Method ◽  
Hplc Method Development ◽  
Development And Validation

The prime aim of the present investigation was to develop and validate a novel, precise, accurate, specific, rapid and economical stability- indicating isocratic reverse phase liquid chromatography method for the quantitative simultaneous estimation of valsartan and hydrochlorothiazide in bulk and marketed formulations. Estimation of drugs in this combination was achieved with a C18 column [Kromasil 100-5 C18 column, P134 250 × 4.6 mm] kept at ambient temperature, isocratic mode using mobile phase of composition acetonitrile and phosphate buffer (40:60 V/V, pH 4). The flow rate was 0.8 ml/min and the effluents were monitored at 235 nm, using variable wavelength UV detector. The retention time of valsartan and hydrochlorothiazide were 2.65 min and 3.97 min, respectively. Validation of the method was done according to the ICH guidelines for different analytical parameters. The method was found to be linear over a range of 50-250 μg/mL for valsartan and hydrochlorothiazide. The established method was as reproducible with a %RSD value of less than 2 and having robustness and accuracy within the specified limits. Assay of marketed formulation was determined and was 99.04% and 99.8% respectively. The stressed samples were analyzed. The proposed method was found to be specific and stability indicating as no interfering peaks of degradation compounds and excipients were noticed. The proposed method can be successfully employed in the estimation of commercial formulations.

Development and Validation of HPLC Method for Simultaneous Estimation of Reduced and Oxidized Glutathione in Bulk Pharmaceutical Formulation

2021 ◽  
Vol 8 (1) ◽  
Author(s):  
Singh N ◽  
◽  
Akhtar MJ ◽  
Anchliya A ◽  
◽  
...  
Keyword(s):  
Detection Limit ◽  
Limit Of Detection ◽  
Reduced Glutathione ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Oxidized Glutathione ◽  
Range Limit ◽  
Limit Of Quantification ◽  
Reduced And Oxidized Glutathione

The objective of this study was the development, optimization, and validation of a RP-HPLC method for the quantification of reduced glutathione (GSH) and oxidized glutathione (GSSG) in pharmaceutical formulations The separation utilized a C18 column at room temperature with absorption wavelength 210nm. The mobile phase was an isocratic flow of a 95:5 (v/v) mixture of 25mM phosphate buffer (pH 2.7) and methanol with flow rate at 1.0 mL/min. Validation of the method assessed with the methods ability in seven categories: linearity, range, limit of detection, limit of quantification, accuracy, precision, and selectivity. The method show an acceptable degree of linearity with r²=0.9994 and 0.999 over a concentration range of 10-200 μg/mL for GSH and GSSG respectively. The detection limit and quantification limit for GSH 20.7μg/mL and 69.24μg/mL and for GSSG 17.22μg/mL and 57.42μg/mL respectively. The percent recovery of the method was 99.98-100.93 %. Following validation, the method was employed in the determination of glutathione in pharmaceutical formulations in the form of a liposome. The proposed method offers a simple, accurate, and inexpensive way to quantify reduced glutathione.

scholarly journals A Stability Indicating Assay Method Development and Validation for the Frovatriptan Succinate Monohydrate by Using UV: A Spectrophotometric Technique

2013 ◽  
Vol 2013 ◽  
pp. 1-6 ◽  
Author(s):  
Hitesh Verma ◽  
Surajpal Verma ◽  
Harmanpreet Singh
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Assay Method ◽  
Forced Degradation ◽  
Solution Stability ◽  
Limit Of Quantification ◽  
Experimental Conditions ◽  
Stability Indicating ◽  
Ich Guidelines ◽  
Relative Standard

A new simple, reliable, inexpensive, and accurate method was developed for the quantification of Frovatriptan Succinate Monohydrate in different physiological media at 244 nm in bulk and in tablet dosage forms. The developed method is an attempt to surpass the disadvantages associated with the reported methods, namely, less sensitive and tedious in usage for routine purposes. Beer’s law was followed over the range of 1.0 µg/mL to 4.5 µg/mL. Stability indicating assay method was developed and validated as per the ICH guidelines using various parameters, for example, accuracy, precision, limit of quantification, limit of detection, robustness, ruggedness, solution stability, recovery, forced degradation (hydrolysis, photo degradation, thermal degradation, and oxidation), and so forth. Percent relative standard deviation associated with all the parameters was less than 2, showing compliance with the acceptance criteria of ICH guidelines. The developed method was very sensitive as limit of quantification and limit of detection were found to be 0.025 µg/mL and 0.00625 µg/mL, respectively. Forced degradation studies of drug reveal good stability under the chosen experimental conditions.

scholarly journals A Stability Indicating UPLC Method for the Determination of Tramadol Hydrochloride: Application to Pharmaceutical Analysis

2012 ◽  
Vol 2012 ◽  
pp. 1-9 ◽  
Author(s):  
Kanakapura B. Vinay ◽  
Hosakere D. Revanasiddappa ◽  
Cijo M. Xavier ◽  
Pavagada J. Ramesh ◽  
Madihalli S. Raghu
Keyword(s):  
Limit Of Detection ◽  
Potassium Dihydrogen Phosphate ◽  
Reversed Phase ◽  
Forced Degradation ◽  
Dihydrogen Phosphate ◽  
Uv Detector ◽  
Limit Of Quantification ◽  
Tramadol Hydrochloride ◽  
Stability Indicating

The use of Ultra Performance Liquid Chromatography (UPLC), with a rapid 5-minute reversed phase isocratic separation on a 1.7 μm reversed-phase packing material to provide rapid ‘‘high throughput’’ support for tramadol hydrochloride (TMH) is demonstrated. A simple, precise and accurate stability-indicating isocratic UPLC method was developed for the determination of TMH in bulk drug and in its tablets. The method was developed using Waters Aquity BEH C18 column (100 mm × 2.1 mm, 1.7 μm) with mobile phase consisting of a mixture of potassium dihydrogen phosphate buffer of pH 2.8 and an equal volume of acetonitrile (60 : 40 v/v). The eluted compound was detected at 226 nm with a UV detector. The standard curve of mean peak area versus concentration showed an excellent linearity over a concentration range 0.5–300 μg mL−1 TMH with regression coefficient (r) value of 0.9999. The limit of detection (S/N =3) was 0.08 μg mL−1 and the limit of quantification (S/N =10) was 0.2 μg mL−1. Forced degradation of the bulk sample was conducted an accordance with the ICH guidelines. Acidic, basic, hydrolytic, oxidative, thermal and photolytic degradation were used to assess the stability indicating power of the method. TMH was found to degrade significantly in acidic, basic and oxidative stress conditions and stable in thermal, hydrolytic and photolytic conditions.

scholarly journals Method Development and Validation of Stability Indicating RP-HPLC Method for Simultaneous Estimation of Escitalopram Oxalate and Clonazepam in Bulk and its Pharmaceutical Formulations

2019 ◽  
Vol 9 (1-s) ◽  
pp. 265-274
Author(s):  
Bindusar Kalia ◽  
Uttam Singh Baghel
Keyword(s):  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Calibration Plot ◽  
Simultaneous Estimation ◽  
Control Analysis ◽  
Reverse Phase ◽  
Limit Of Quantification ◽  
Rp Hplc

This article refers to simple isocratic reverse-phase high-performance liquid chromatographic method (RP-HPLC) developed for the simultaneous quantification of Escitalopram Oxalate (EST) and Clonazepam (CZP) in active pharmaceutical ingredient and pharmaceuticals. The separation of the two drugs was attained using a C₁₈ column (250mm×4.6mm, 5µ) as a stationary phase. The mobile phase was used as a mixture of methanol; acetonitrile; and 0.05M potassium dihydrogen orthophosphate buffer (pH 4 adjusted by orthophosphoric acid) with an isocratic ratio of 40:20:40 v/v. Detection was made by using PDA detector at 210 nm. Escitalopram Oxalate (RT= 4.428 minutes) and Clonazepam (RT= 6.532 minutes) were separated in a single chromatographic run with resolution of 8.719. The calibration plot indicated good linear relationship with r2 = 0.998 for Escitalopram Oxalate in concentration range of 32 µg/ml - 48 µg/ml and r2 = 0.999 for Clonazepam in concentration range of 16 µg/ml - 24 µg/ml. The retrievals for Escitalopram Oxalate and Clonazepam were found to be 99.75% and 99.00%, respectively. The established analytical method was validated and found acceptable as per ICH guidelines for linearity, precision, accuracy, specificity, limit of detection, limit of quantification, robustness and stability. Escitalopram Oxalate and Clonazepam individually as well as in combination were exposed to different stress conditions like acid, base, thermal, photolytic and oxidation degradation and peaks of a degraded product were well determined from peaks of pure drug. This method is modest, quick and appropriate for routine quality control analysis. Keywords: Reverse Phase – HPLC; Escitalopram Oxalate; Clonazepam; Validation; Degradation study.

scholarly journals RP-HPLC Method Development and Validation for the Estimation of Mirabegron in Bulk and Dosage Form

2020 ◽  
Vol 10 (1) ◽  
pp. 31-38
Author(s):  
Rahul Suryawanshi ◽  
Siddiqua Shaikh ◽  
Snehal Patil
Keyword(s):  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Limit Of Quantification ◽  
Rp Hplc ◽  
Hplc Method Development ◽  
Tablet Dosage

A new, simple, precise, accurate and reproducible Reverse Phase High Performance Liquid Chromatography (RP-HPLC) method for Simultaneous estimation of bulk and pharmaceutical formulations. Separation of Mirabegron was successfully achieve , C18, 250X4.6mm, 5µm or equivalent in an isocratic mode utilizing methanol water (70:30) at pH 5.0 Adjusted to OPA at a flow rate of 1.0ml/min and eluate was monitored at 243nm, with a retention time of 2.584 minutes for Mirabegron. The method was validated and the response was found to be linear in the drug concentration range of 50µg/ml to150 µg/ml for Mirabegron. The values of the correlation coefficient were found to 0.999for Mirabegron. The Limit of Detection(LOD) and Limit of Quantification (LOQ) for Mirabegron were found to be 0.149 and 0.498 respectively. This method was found to be good percentage recovery were found to be 99 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 International Council for Harmonisation(ICH) guidelines for Linearity, Accuracy, Precision, Specificity and

A new stability indicating chiral RP-HPLC method for determination of degradation products in Meclizine Hydrochloride

2020 ◽  
Vol 16 ◽  
Author(s):  
Bryan Gowramma ◽  
Ramachandran Senthil Kumar ◽  
Kaviarasan Lakshmanan ◽  
Rajagopal Kalirajan ◽  
Subramanian Nainar Meyyanathan
Keyword(s):  
Limit Of Detection ◽  
Degradation Products ◽  
Pharmaceutical Preparations ◽  
Hplc Method ◽  
Stress Conditions ◽  
Main Peak ◽  
Uv Detector ◽  
Limit Of Quantification ◽  
Degradation Behaviour ◽  
Stability Indicating

Background: An enantiomeric separation of stability-indicating high-performance liquid chromatographic method was developed and validated for the analysis of Meclizine enantiomers. The degradation behaviour of Meclizine Hydrochloride was investigated under different stress conditions recommended by International Conference on Harmonization (ICH). Experiment: Enantiomeric resolution of the drug and complete separation from its degradation products were successfully achieved on a Phenomenex® lux cellulose 1 C18 (250 mm × 4.6 mm i.d, 5 µm particle size) column, using UV detector at a wavelength of 230 nm, with mobile phase consisting of acetonitrile, 20mM ammonium bicarbonate at the ratio of 75:25 (v/v), and a flow rate of 1 mL/min. The drug was subjected to alkaline, acidic, neutral, oxidative and photolytic conditions in order to mimic stress conditions. Result: The degradation products were well resolved from main peak and proving the stability-indicating power of the method. The developed method provided linear responses within the concentration range 1-5 µg/mL, and regression analysis showed a correlation coefficient value (r2) of 0.999. The HPLC method was validated as per ICH guidelines with respect to specificity, precision, linearity and robustness. Limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.25 µg/mL and 1.00 µg/mL respectively. Conclusion: The method provides good sensitivity and excellent precision and reproducibility. The method was highly selective, where degradation products and co formulated compounds did not interfere. The proposed method was successfully applied in pharmaceutical preparations.

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