scholarly journals “Robust and Rapid” UV Spectroscopic Method for Estimation of Luliconazoleand Clobetasol Propionate Drug Combination

2021 ◽  
pp. 313-320
Author(s):  
Binal Solanki ◽  
Hirak Joshi
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Spectroscopic Method ◽  
Research Work ◽  
Clobetasol Propionate ◽  
New Combination ◽  
Simultaneous Estimation ◽  
Statistical Validation ◽  
Limit Of Quantification ◽  
Laboratory Procedure

Objective: The new combination for Luliconazole and Clobetasol Propionate was approved for the treatment of variety of skin disease. The main objective of this research is development and validation of novel, simple, fast and responsive derivative spectroscopic process for simultaneous estimation of newly approved combination Luliconazole (LLZ) and Clobetasol Propionate (CLP). Methodology: Here in this first derivative spectroscopic method, the absorbance of LLZ and CLP was taken at 312nm (ZCP of CLP) and 249nm (ZCP of LLZ) respectively. Establishment of linearity was in a concentration varies from 10-50 µg/ml for Luliconazole and 5-25µg/ml for Clobetasole Propionate. Results: From the method developed above the R2 value observed for LLZ and CLP is 0.9988 and 0.9961. Statistical validation of accuracy and reproducibility was done for planned procedure with the help of recovery studies. The mean % recovery of Luliconazole and Clobetasol Propionate was found to be 99.45 % and 99.43% respectively. For LLZ the Limit of detection is 0.0054 µg/ml and limit of quantification is 0.0164 µg/ml and for CLP the Limit of detection is 0.0009µg/ml and limit of quantification 0.0027µg/ml. Conclusion: From research work the method development was done and shows fast, precise, exact and easily accessible laboratory procedure for routine evaluation of combination drugs.

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 Development and Validation of a Green Analytical Method for the Determination of Aspirin and Domperidone Bulk or Formulation Using UV and HPLC

2020 ◽  
Vol 10 (6) ◽  
pp. 49-56
Author(s):  
Sneha Jagnade ◽  
Pushpendra Soni ◽  
Lavakesh Kumar Omray
Keyword(s):  
Analytical Method ◽  
Method Development ◽  
Limit Of Detection ◽  
Research Work ◽  
Ultra Violet ◽  
Limit Of Quantification ◽  
Intermediate Precision ◽  
Rp Hplc ◽  
Development And Validation

The aim of present study was to investigate the development and validation of a green analytical method for the determination of aspirin and domperidone. Method Development and Validation for Estimation of Domperidone and Aspirin in bulk or formulation by using RP-HPLC. The RP-HPLC method was developed for estimation of Aspirin and Domperidone in synthetic mixture by isocratically using 10 mM KH2PO4: Acetonitrile (20:80) as mobile phase, Prontosil C-18 column (4.6 x 250 mm, 5μparticle size) column as stationary phase and chromatogram was recorded at 231 nm. Then developed method was validated by using various parameters such as, linearity, Range accuracy, precision repeatability, intermediate precision, robustness, limit of detection, limit of quantification. The proposed methods were found to be linear with correlation coefficient close to one. Precision was determined by repeatability, Intermediate precision and reproducibility of the drugs. The robustness of developed method was checked by changing in the deliberate variation in solvent. The result obtained shows the developed methods to be Cost effective, Rapid (Short retention time), Simple, Accurate (the value of SD and % RSD less than 2), Precise and can be successfully employed in the routine analysis of these drugs in bulk drug as well as in tablet dosage form. The Simplicity, Rapidly and Reproducibility of the proposed method completely fulfill the objective of this research work. Keywords: Asprin; Domperidone; HPLC; Ultra Violet; Validation

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

HPTLC METHOD DEVELOPMENT AND VALIDATION FOR SIMULTANEOUS ESTIMATION OF CHLORTHALIDONE AND IRBESARTAN IN COMBINED TABLET DOSAGE FORM

INDIAN DRUGS ◽  
2014 ◽  
Vol 51 (07) ◽  
pp. 46-52
Author(s):  
P Kalaiselvi ◽  
◽  
K. G. Lalitha
Keyword(s):  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Ammonia Solution ◽  
Dosage Forms ◽  
Simultaneous Estimation ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Tablet Dosage ◽  
Hptlc Method

A simple, accurate and rapid high performance thin layer chromatography (HPTLC)-densitometry method was developed for separation and determination of chlorthalidone (CHL) and irbesartan (IBS) in pharmaceutical dosage forms. The compounds were separated on silica gel 60 GF254, HPTLC plates using mobile phase of toluene: ethyl acetate: acetonitrile: methanol: ammonia solution (25%) [5:2:2:1:0.2 v/v/v/v] as compact spots at Rf of 0.57 for chlorthalidone and Rf of 0.36 for irbesartan. Densitometric detection was performed at 254 nm. The method was validated in terms of linearity, precision, accuracy, limit of detection (LOD), and limit of quantification (LOQ). The calibration curves were linear in the range of 12.5-75 ng/spot for CHL and 150-900ng/spot for IBS. For CHL recovery varied in range of 99.26-101.25% and for IBS recovery varied in range of 99.76-100.40%. The LOD was found 1.33 and 11.34 ng/spot for CHL and IBS respectively. The LOQ was found 4.03 and 14.37 ng /spot for CHL and IBS respectively. It was observed that the proposed HPTLC method could be used for efficient analysis of the CHL and IBS in combined tablet dosage forms.

METHOD DEVELOPMENT AND VALIDATION OF UV SPECTROPHOTOMETRIC AND STABILITY INDICATING RP-HPLC METHODS FOR SIMULTANEOUS ESTIMATION OF MOXIFLOXACIN HYDROCHLORIDE AND KETOROLAC TROMETHAMINE IN BULK AND OPTHALMIC DOSAGE FORMS

INDIAN DRUGS ◽  
2017 ◽  
Vol 54 (04) ◽  
pp. 38-46
Author(s):  
H Parimi ◽  
C Bolla ◽  
B. M. Gandhi ◽  
B. R Vatchavai ◽  
S. S Kamatham ◽  
...  
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Dosage Forms ◽  
Simultaneous Estimation ◽  
Uv Spectrophotometry ◽  
Ketorolac Tromethamine ◽  
Limit Of Quantification ◽  
Stability Indicating ◽  
Rp Hplc

The main objective of the present work was to develop a simple, precise, accurate and reproducible UV-Spectrophotometric and stability indicating RP-HPLC methods for simultaneous estimation of moxifloxacin HCl (MOX) and ketorolac tromethamine (KET) in bulk and ophthalmic dosage forms. UV Spectrophotometry was carried out by simultaneous equation method using distilled water : acetonitrile (50:50 V/V) as solvent. The wavelengths were found to be 295 nm for MOX and 322 nm for KET. The isobestic point was found to be 308 nm. The linearity range is 2-10 μg/mL for both MOX and KET with correlation co-efficient >0.99. The separation of these two drugs using RP-HPLC was achieved on a SHISHEDO C18, 250×4.6 mm, 5 micron size column with a mobile phase consisting of acetonitrile and acetate buffer (45:55 V/V) at pH 4.0 at a flow rate of 1 mL/min and UV detection at 308 nm. The retention times were observed to be 2.418 and 3.827 minutes for MOX and KET, respectively. Linearity was found to be 10-50 μg/mL for both MOX and KET, respectively. The two developed methods were successfully validated for accuracy, precision, linearity, limit of detection, limit of quantification and robustness. The two developed methods were validated according to ICH guidelines and were found to be with in the limits. The stress testing of the drugs individually was carried out under acidic, alkaline, oxidation, photo-stability and thermal degradation conditions and its degradation products were studied. These two methods could be used for simultaneous estimation of MOX and KET in bulk and ophthalmic dosage forms.

scholarly journals Method Development and Validation for Simultaneous Determination of Ezetimibe and Simvastatin In Combined Pharmaceutical Dosage Form By RP-HPLC Method

2013 ◽  
Vol 2 (2) ◽  
pp. 60-69 ◽  
Author(s):  
G Krishnaveni ◽  
PVV Sathyannarayana
Keyword(s):  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Simultaneous Estimation ◽  
Internal Diameter ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms

A simple, rapid reverse phase high-performance liquid chromatographic method was developed and validated for the simultaneous estimation of Ezetimibe and Simvastatin in bulk and pharmaceutical dosage forms. Chromatography was carried out by using Chromosil C-18,column having 250 x 4.6mm internal diameter with a mixture of Methanol:Acetonitrile:0.1%Orthophosphoric Aid in the ratio of 75:20:05 (v/v/v) as mobile phase. Determination of the different analytical parameters such as linearity, precision, accuracy, and specificity, limit of detection (LOD) and limit of quantification (LOQ) was done. The calibration curve was found to be linear for each analyte in the desired concentration range. The average recovery was found to be 99.88 and 100.12 for Ezetimibe and Simvastatin respectively. The proposed method is highly sensitive, precise and accurate, which was evident from the LOD value of 1.2ppm and 0.25ppm for Ezetimibe and Simvastatin respectively and hence the present method can be applied successfully for the quantification of active pharmaceutical ingredient (API) content in the combined formulations of Ezetimibe and Simvastatin. DOI: http://dx.doi.org/10.3329/ijpls.v2i2.15450 International Journal of Pharmaceutical and Life Sciences Vol.2(2) 2013: 60-69

scholarly journals UV Spectrophotometric Methods to Quantify Alogliptin Benzoate and Pioglitazone Hydrochloride

2021 ◽  
pp. 31-41
Author(s):  
Dhanya B. Sen ◽  
Ashim K. Sen ◽  
Aarti S. Zanwar ◽  
Harshita Pandey ◽  
Rajesh A. Maheshwari
Keyword(s):  
Limit Of Detection ◽  
Spectroscopic Method ◽  
Simultaneous Estimation ◽  
Control Analysis ◽  
Limit Of Quantification ◽  
Spectrophotometric Methods ◽  
First Derivative ◽  
Ich Guidelines ◽  
The Difference ◽  
Tablet Dosage

Three new, precise, accurate and sensitive UV-Spectrophotometric methods namely Ratio Difference Spectroscopic Method (RDSM), First Derivative of Ratio Spectra Method (DR1) and Area Under Curve Method (AUC) were developed and validated for simultaneous assessment of alogliptin benzoate (ALO) and pioglitazone hydrochloride (PIO) in tablet dosage form. In RDSM, ratio spectra of both the drugs were recorded by dividing the mixtures using interfering drug as divisor. Then the difference between the amplitudes of obtained ratio spectra was measured at 288 and 291 nm for ALO and 236 and 245 nm for PIO. The second method DR1, where the first derivative of ratio spectra of both the drugs were recorded and the first derivative signal was measured at 290 nm for ALO and 276.8 nm for PIO. The scaling factor was fixed as 1 and wavelength interval (Δλ) as 2 for recording the first derivative of ratio spectra.  In the third method (AUC), peak area of recorded zero order spectra was measured at 276 ± 10 nm for ALO and 267.8 ± 10 nm for PIO. All three proposed methods were validated according to “International Conference on Harmonization” (ICH) guidelines parameters. For all three methods, ALO and PIO obeyed Beer’s law in the range of 0.5-5 & 1.8-18 µg/ml, respectively. The % RSD of repeatability of measurement, intra-day and inter-day precision were found to be less than 2 for all three methods. Limit of detection (LOD) and Limit of quantification (LOQ) of the drugs were calculated which proved the sensitivity of the methods. The accuracy ranged between 98-101% for all three methods. No interference from pharmaceutical excipients present in the formulation was observed.  These proposed methods were found to be simple, sensitive, accurate and precise and can be applied to the simultaneous estimation of ALO and PIO in combined tablet formulation and also appropriate for routine quality control analysis.

scholarly journals Method Development and Its Validation for Simultaneous Estimation of Domperidone and Esomeprazole by RP-HPLC in Combination Tablet Dosage Form

2016 ◽  
Vol 1 (01) ◽  
pp. 46-55
Author(s):  
V. Tejasvi Reddy ◽  
S. Hari Hara Kumar ◽  
M Akiful Haque ◽  
Vasudha Bakshi
Keyword(s):  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Potassium Dihydrogen Phosphate ◽  
Correlation Coefficients ◽  
Simultaneous Estimation ◽  
Dihydrogen Phosphate ◽  
Limit Of Quantification ◽  
Combination Tablet ◽  
Rp Hplc

A simple and validated reverse phase high performance liquid chromatography (RP-HPLC) method was developed for simultaneous estimation of Esomeprazole and Domperidone. Different HPLC Chromatographic conditions were used to find out the optimum chromatographic condition for best elution of drugs. Good chromatographic separation was achieved on Develosil ODS HG-5 RP C18 (15cmX4.6mm, 5m Particle size), analytical column using a mixture of Potassium dihydrogen phosphate buffer pH: acetonitrile in the ratio of 45:55 v/v used as mobile phase at the flow rate of 1 ml/min and detector wavelength at 284nm. The validation of the proposed method was carried out for specificity, linearity and range, accuracy, precision, limit of detection and limit of quantification. Linearity range was found to be 0-140 μg/ml and 0-150 μg/ml with correlation coefficients of 0.995 and 0.994 and retention time of 2.59 and 3.85 min for Domperidone and Esomeprazole respectively. The LOD was found to be 0.341 g/ml and 2.031 g/ml and LOQ was found to be 1.023 g/ml and 6.093 g/ml respectively. The result shows the developed method is yet another suitable method for assay and stability studies which can help in the analysis of Domperidone and Esomeprazole in different formulations.

scholarly journals Ultra Sensitive UPLC Method Development and Validation for the Simultaneous Estimation of Tamsulosin Hydrochloride and Tolterodine Tartrate in Bulk and Pharmaceutical Dosage Form

2018 ◽  
pp. 50-59
Author(s):  
Mahmoud M. Sebaiy ◽  
Sobhy M. El-Adl ◽  
Mohamed Baraka ◽  
Mostafa S. Mohram ◽  
Fatma Ibrahim
Keyword(s):  
Dosage Form ◽  
Method Development ◽  
Limit Of Detection ◽  
Pharmaceutical Preparation ◽  
Potassium Phosphate ◽  
Reversed Phase ◽  
Simultaneous Estimation ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Significant Difference

A rapid, sensitive and accurate ultra-performance reversed phase liquid chromatographic method was developed for the simultaneous determination of tamsulosin and tolterodine in pure form and pharmaceutical preparation. The developed UPLC method is superior to conventional HPLC with respect to speed, resolution, solvent consumption and cost. The separation was carried out on RP C18 nucleosil (1.7 µm, 5 cm x 2 mm) using an isocratic mode in eluting Tamsulosin and Tolterodine at 1.54 min and 2.43 min respectively with a mobile phase composed of acetonitrile and 0.025N potassium phosphate buffer pH 3.50 (60%:40%), respectively. Chromatographic run time was 5 min with a flow rate 0.5 ml/min and UV detection at 220 nm. The linearity for tamsulosin and tolterodine were in the range of 2-20 µg/mL for both drugs, showed excellent recoveries for bulk and tablet dosage form with a very low LOD of 4.29 and 0.59 ng/mL for tamsulosin and tolterodine, respectively. The method has been validated for linearity, accuracy, precision, specificity, and limit of detection, limit of Quantification, robustness, and ruggedness. The method which was developed was validated as per the ICH guidelines. Finally, the method was compared statistically with reference methods indicating that there is no significant difference between them in respect of precision and accuracy.

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