SIMULTANEOUS ESTIMATION OF BERBERINE HYDROCHLORIDE AND INDOMETHACIN FOR IN VITRO DIFFUSION PROFILE BY UV SPECTROSCOPY

INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (02) ◽  
pp. 26-30
Author(s):  
Shaily Lalka ◽  
Munira Momin ◽  
Atul Sherje ◽  
Keyword(s):  
Limit Of Detection ◽  
Uv Spectroscopy ◽  
Diffusion Profile ◽  
Simultaneous Estimation ◽  
Limit Of Quantification ◽  
Berberine Hydrochloride ◽  
Ich Guidelines ◽  
Relative Standard ◽  
Gel Formulations

The present work aims to develop a precise, accurate and validation method to estimate berberine hydrochloride and indomethacin in gel formulations. In the present work, 50% phosphate buffer pH 7.4, 25% methanol and 25% ethanol blend was used as a solvent to increase the solubility of both the drugs. The analytical wavelength for berberine hydrochloride and indomethacin was 343 nm and 316nm, respectively. The method was validated for linearity, accuracy, precision, limit of detection, limit of quantification and robustness as per the ICH guidelines. The validated method was then applied in the diffusion study of the drugs from two different gel formulations. Beer’s law was obeyed in the concentration range of 4-14 µg/ml and 10-60 µg/ml for berberine hydrochloride and indomethacin, respectively. The method was found to be accurate and precise with relative standard deviation within 2% as per the ICH guidelines.

scholarly journals COMPARISON OF RP-HPLC AND UV SPECTROPHOTOMETRIC METHODS FOR ESTIMATION OF HALOPERIDOL IN PURE AND PHARMACEUTICAL FORMULATION

2018 ◽  
Vol 8 (5-s) ◽  
pp. 277-282 ◽  
Author(s):  
AK Jain ◽  
BK Dubey ◽  
D Basedia ◽  
S Dhakar ◽  
M Ahirwar ◽  
...  
Keyword(s):  
Limit Of Detection ◽  
Uv Spectroscopy ◽  
Pharmaceutical Formulation ◽  
In Vitro Dissolution ◽  
Uv Spectrophotometry ◽  
Limit Of Quantification ◽  
Spectrophotometric Methods ◽  
Rp Hplc ◽  
Relative Standard

An accurate, precise, sensitive and reproducible High-performance liquid chromatographic (HPLC) and UV spectrophotometric methods were developed and validated for the quantitative determination of haloperidol (HPD) in bulk drug and pharmaceutical formulation. Different analytical performance parameters such as linearity, precision, accuracy, specificity, limit of detection (LOD) and limit of quantification (LOQ) were determined according to International Conference on Harmonization ICH Q2B guidelines. The RP-HPLC method was developed by the isocratic technique on a reversed-phase Thermo C18 (250 × 4.6 mm, 5µm) column with mobile phase consisting of Methanol: Acetonitrile (50:50v/v) at flow rate of 1.0 ml/min. The retention time for HPD was 2.238±0.3min. The UV spectrophotometric determinations were performed at 244 nm using 80% methanol as a solvent. The linearity range for HPD was 5-25 μg/ml for both HPLC and UV method. The linearity of the calibration curves for each analyte in the desired concentration range was good (r2 >0.999) by both the HPLC and UV methods. The method showed good reproducibility and recovery with percent relative standard deviation less than 2%. Moreover, the accuracy and precision obtained with HPLC co-related well with the UV method which implied that UV spectroscopy can be a cheap, reliable and less time consuming alternative for chromatographic analysis. The proposed methods are highly sensitive, precise and accurate and hence successfully applied for determining the assay and in vitro dissolution of a marketed formulation. Keywords: HPLC, UV Spectrophotometry, Haloperidol, Pharmaceutical formulation, Method validation, Quantitative analysis

Liquid Chromatographic analysis of Methotrexate and Minocycline- Relevance to the determination in Plasma/Nanoparticulate formulations

2021 ◽  
Vol 08 ◽  
Author(s):  
Kumar Janakiraman ◽  
Venkateshwaran Krishnaswami ◽  
Vaidevi Sethuraman ◽  
Vijaya Rajendran ◽  
Ruckmani Kandasamy
Keyword(s):  
Limit Of Detection ◽  
Biological Fluids ◽  
In Vitro Release ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Limit Of Quantification ◽  
Simple Method ◽  
Relative Standard ◽  
Validation Parameters

Aim: To develop an RP-HPLC method for the simultaneous estimation of methotrexate (MTX) and minocycline (MNC). Background: Different HPLC methods were reported for the estimation of MTX/MNC individually, but there is no report for the simultaneous estimation of both MTX and MNC in a simple method. Objective: The objective of the developed method is to utilize the method for the estimation of MTX/MNC in different pharmaceutical formulations and in biological fluids. Methods: An HPLC method for the estimation of methotrexate (MTX) and minocycline (MNC) relevance to the evaluation of nanoparticulate formulations has been developed and validated. Chromatographic estimation was achieved using the mobile phase composition of sodium acetate buffer and acetonitrile (70:30% v/v) at pH 4.0 at a flow rate of 0.2 mL/min at 307 nm. Results: The calibration curve for MTX and MNC was found to be linear at nanogram (5 to 25 ng.mL-1) and microgram (5 to 25 μg.mL-1) levels at a correlation coefficient range of 0.98 to 0.99 for both MTX/MNC. The lower limit of detection and limit of quantification were found to be 0.026 ng.mL-1 and 0.079 ng.mL-1 for MTX and MNC, respectively. The percentage relative standard deviation for validation parameters of both drugs was found to be less than 6.5%. The amount of MTX and MNC present within the nanoparticles was found to be MTX (0.84 mg/mL) and MNC (0.61 mg/mL). The in vitro release showed an immediate release pattern for MTX (64.95±2.08%) and MNC (90.90±1.78%) within 12 h. Conclusion: The developed analytical method for the simultaneous estimation of MTX and MNC was found to be simple, affordable, dynamic, low cost, rapid and easy to perform with good repeatability. This method is also time consuming, since the peaks were obtained within a moderate analysis time.

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.

METHOD DEVELOPMENT AND VALIDATION FOR THE SIMULTANEOUS ESTIMATION OF THYMOL AND EUGENOL BY USING RP-HPLC IN PURE AND IN EMULGEL FORMULATION

INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (07) ◽  
pp. 59-65
Author(s):  
Vinita C. Patole ◽  
Shilpa P. Chaudhari ◽  
Keyword(s):  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Peak Areas ◽  
80 A 20 ◽  
Development And Validation

An attempt was made to develop a simple, selective, rapid and precise high-performance liquid chromatography (HPLC) method for simultaneous estimation of thymol and eugenol. Analysis was performed on a C18 column with the mobile phase consisting of solvent %A (water) and solvent %B (acetonitrile) with the following gradient: 0–1 min, 80 % A, 20 % B; 1–7 min, 40 % A and 60 % B; 7–12 min, 10 % A and 90 % B; and 12–15min, 80 % A and 20 % B at a flow rate of 0.6 mL/min. The compounds were well separated on a Thermo Scientific Hypersil BDS RP C18 column (4.6 mm × 150 mm, dp = 5 µm) and ultraviolet detection at 280 nm. The retention times of eugenol and thymol were 10.5 min and 11.6 min, respectively. Validation of the proposed method was carried out according to the guidelines of the International Council on Harmonization (ICH). The linearity of the method is good for thymol and eugenol over the concentration range of 1–50 ppm, and the r 2 values were 0.9996 for both thymol and eugenol. The calculated limit of detection (LOD) value was 0.5ppm and the limit of quantification (LOQ) value was 1ppm for both the analytes. The intra and interday relative standard deviation (RSD) of the retention time and peak areas was less than 3 %.The established method was appropriate, and the two markers were well resolved, enabling efficient quantitative analysis of thymol and eugenol.

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.

scholarly journals DEVELOPMENT AND EVALUATION OF NOVEL ESTIMATION TECHNIQUES FOR IN VITRO DISSOLUTION STUDY AND VALIDATION PROTOCOL FOR ESCITALOPRAM AS ANTIDEPRESSANT DRUG AND THEIR FORMULATION

2020 ◽  
pp. 55-61
Author(s):  
SHRIRAM H. BAIRAGI ◽  
R. S. GHOSH
Keyword(s):  
Limit Of Detection ◽  
Antidepressant Drug ◽  
Correlation Factor ◽  
In Vitro Dissolution ◽  
Linear Calibration ◽  
Limit Of Quantification ◽  
Minimum Concentration ◽  
Dissolution Study ◽  
Relative Standard

Objective: To develop and validate the RP-HPLC method and in vitro dissolution study for escitalopram as antidepressant drug and their formulation. Methods: The chromatographic separation was done by using a C-18, 150 mm column and a mobile phase consisting of phosphate buffer (40%) and acetonitrile HPLC grade (60%). Detection was carried out at 211 nm with a flow rate of 1 ml/min with an injection of 20 μl. The method was validated with different parameters such as linearity, precision, accuracy, robustness, and limit of detection (LOD), the limit of quantification (LOQ) according to ICH guidelines. Results: The linear calibration curve was obtained in the concentration range of 0-50 μg/ml and gave an average correlation factor 0.992. The retention time was observed at 2.96 min. The Minimum concentration level at which the analyte can be reliably detected (LOD) and quantified (LOQ) were found to be 0.03 and 0.09 µg/ml, respectively. The relative standard deviation of intra and the inter-day assay was found to be less than 2. The dissolution studies show moderate dissolution (23.4%) after 45 min, but it reaches a plateau after approximately 25 min. Conclusion: This method was found to be simple, rapid and economic with less run time. The validated parameters manifest the method is reliable, linear, accurate and precise as well as robust with minor variations in chromatographic parameters. Therefore, the developed method can be applied for both routine analysis and quality control assay and it could be a very powerful tool to investigate the stability of escitalopram.

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 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 Rapid, Simple, and Sensitive Spectrofluorimetric Method for the Estimation of Ganciclovir in Bulk and Pharmaceutical Formulations

2013 ◽  
Vol 2013 ◽  
pp. 1-5 ◽  
Author(s):  
Garima Balwani ◽  
Emil Joseph ◽  
Satish Reddi ◽  
Vibhu Nagpal ◽  
Ranendra N. Saha
Keyword(s):  
Standard Deviation ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Calibration Graph ◽  
Limit Of Quantification ◽  
Average Percentage ◽  
Ich Guidelines ◽  
Spectrofluorimetric Method ◽  
Relative Standard

A new, simple, rapid, sensitive, accurate, and affordable spectrofluorimetric method was developed and validated for the estimation of ganciclovir in bulk as well as in marketed formulations. The method was based on measuring the native fluorescence of ganciclovir in 0.2 M hydrochloric acid buffer of pH 1.2 at 374 nm after excitation at 257 nm. The calibration graph was found to be rectilinear in the concentration range of 0.25–2.00 μg mL−1. The limit of quantification and limit of detection were found to be 0.029 μg mL−1and 0.010μg mL−1, respectively. The method was fully validated for various parameters according to ICH guidelines. The results demonstrated that the procedure is accurate, precise, and reproducible (relative standard deviation <2%) and can be successfully applied for the determination of ganciclovir in its commercial capsules with average percentage recovery of 101.31 ± 0.90.

Simultaneous Estimation of Apremilast and Betamethasone Dipropionate in Microsponge-Based Topical Formulation using a Stability Indicating RP-HPLC Method: A Quality-by-Design Approach

2021 ◽  
Author(s):  
Prashansha Mullick ◽  
Sadhana P Mutalik ◽  
Aswathi R Hegde ◽  
Abhijeet Pandey ◽  
P C Jagadish ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Limit Of Detection ◽  
Betamethasone Dipropionate ◽  
Simultaneous Estimation ◽  
Topical Formulation ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Column Temperature ◽  
Stability Indicating ◽  
Relative Standard

Abstract A stability-indicating reverse phase high-performance liquid chromatography method was developed and validated for simultaneous quantification of apremilast (APL) and betamethasone dipropionate (BD) in bulk as well as drug loaded microsponges. Various mobile phase systems were screened to check the system suitability followed by force degradation analysis to determine APL and BD stability under varying stress conditions. A central composite design model was used to optimize the column temperature and flow rate using Design Expert® (9.0.1). One factor at a time approach with five independent factors were used to validate the robustness of the method. Finally, APL and BD were precisely and accurately quantified from drug loaded microsponges using the validated method. A favorable separation of APL and BD was obtained on a Phenomenex® Luna C18 column using a mixture of 50 mM phosphate buffer containing 0.1% triethylamine (pH 6.1) and acetonitrile (60:40%v/v) as mobile phase. Both the drugs were found to be stable when exposed to stressors such as heat-, light-, alkali-, acid- and peroxide-induced degradation. The calibration curves were found to be linear with appreciable limit of detection and limit of quantification. Recovery and percentage relative standard deviation of peak areas for APL and BD were found to be &lt; 2.0% and 99–100% in bulk drug solution and &lt;2.0% and 99–103% in microsponge formulation, respectively. Statistical analysis using analysis of variance indicated that the model was significant (P &lt; 0.001). Hence, the developed method can be effectively used to quantify APL and BD, both in bulk as well as microsponge formulations.

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