scholarly journals Chemometric Access for RP-HPLC Simultaneous Estimation of Tadalafil and Dapoxetine Applying Response Surface Methodology

2021 ◽  
pp. 278-288
Author(s):  
S. Jayaseelan ◽  
N. Kannappan ◽  
V. Ganesan
Keyword(s):  
Response Surface Methodology ◽  
Response Surface ◽  
Flow Rate ◽  
Phosphate Buffer ◽  
Desirability Function ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Statistical Experimental Design ◽  
Good Resolution ◽  
Rp Hplc

Aims: A RP-HPLC method was developed and validated for simultaneous estimation of Tadalafil and Dapoxetine applying statistical experimental design. Methodology: Multivariate optimization of the experimental conditions of RP-HPLC method was using Design of experiments. Independent three factors like phosphate buffer pH, mobile phase composition and flow rate were applied to design mathematical models. To study the response surface methodology by using Central composite design (CCD). In depth the effects of these independent factors was studied using CCD. Simultaneously optimize the retention time and resolution of the analytes was applying Desirability function. Results: The predicted and optimized data from contour picture containing phosphate buffer (pH 3.4) and acetonitrile in the ratio of 40:60%v/v respectively. Flow rate was found to be 0.8 ml/min. Baseline separation of both analytes with run time of less than 10.0 min and good resolution were achieved using these optimum conditions. Conclusion: Method was validated according to ICH guidelines by using optimized assay conditions. Therefore, the reports distinctly indicated that Quality by design access could be satisfactorily used to optimize RP-HPLC method for simultaneous estimation of Tadalafil and Dapoxetine.

Box-Behnken Design-Desirability Function Approach in Optimization of HPLC Method for Simultaneous Determination of Ibuprofen Along with Additives in Syrup Formulation

2020 ◽  
Author(s):  
Şule Dinç-Zor ◽  
Özlem Aksu Dönmez
Keyword(s):  
Simultaneous Determination ◽  
Flow Rate ◽  
Sodium Benzoate ◽  
Desirability Function ◽  
Hplc Method ◽  
Analysis Time ◽  
Statistical Experimental Design ◽  
Good Resolution ◽  
Sunset Yellow

Abstract Background The advantages of simultaneous analyses are a decrease in analysis time and a more economical use of solvents and reagents. It is desirable that HPLC analyses possess both short term and good resolution. Objective The aim of the current study is to develop an HPLC method for the simultaneous determination of ibuprofen, sodium benzoate, methyl paraben and propyl paraben as preservatives, and sunset yellow as a colorant, in syrup formulation. Method To optimize chromatographic separation conditions, multi-response optimization using the Derringer’s desirability function was employed for the development of a rapid and efficient HPLC method. The ranges of independent variables used for the optimization process were 50–60% (v/v) for acetonitrile, 5.0–7.0 for pH, and 1.0–2.0 mL/min for flow rate of the mobile phase. The effects of these variables on the output responses, such as critical resolution between sunset yellow and sodium benzoate and retention time of the last peak indicating analysis time of the method, were evaluated by statistical experimental design. Results Optimum conditions fixed for the simultaneous analyses were acetonitrile:phosphate buffer (60:40, v/v), pH 5.0, and a flow rate of 1.8 mL/min. The eluate was monitored using a photo diode detector set at 220 nm. Total chromatographic analysis time was approximately 3 min. Conclusions The developed method validated as per International Conference on Harmonization guidelines was successfully applied for the determination of five compounds in their pharmaceutical formulation. Highlights This efficient method has isocratic elution system and can be used for routine analyses of these compounds in similar pharmaceutical products.

scholarly journals A Validated RP – HPLC Method for Simultaneous Estimation of Cefixime and Cloxacillin in Tablets

2008 ◽  
Vol 5 (3) ◽  
pp. 648-651 ◽  
Author(s):  
G. Rathinavel ◽  
P. B. Mukherjee ◽  
J. Valarmathy ◽  
L. Samueljoshua ◽  
M. Ganesh ◽  
...  
Keyword(s):  
Flow Rate ◽  
Retention Time ◽  
Phosphate Buffer ◽  
Mobile Phase ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Rp Hplc

This paper presents a RP-HPLC method for the simultaneous estimation of cefixime and cloxacillin in tablets. The process was carried out on C18column (5 μm, 25 cm × 4.6 mm, i.d) using phosphate buffer (pH 5.0), acetonitrile and methanol in the ratio 80:17:3 respectively as a mobile phase at a flow rate of 2mL/min. Wavelength was fixed at 225 nm. The retention time of cefixime and cloxacillin was found to be 5.657 and 6.200 min, respectively. The developed method is rapid and sensitive and it can be used for estimation of combination of these drugs in tablets.

scholarly journals RP-HPLC Method for Determination of Salbutamol and Bromhexine in Syrup: Modelling and Optimization by Response Surface Methodology

2020 ◽  
Vol 32 (12) ◽  
pp. 3135-3143
Author(s):  
Chung Duong Dinh ◽  
Yen Nguyen Ngoc Thi ◽  
Khanh Quan Nguyen Huu ◽  
Duy Chinh Nguyen ◽  
Ung Thanh Dat ◽  
...  
Keyword(s):  
Response Surface Methodology ◽  
Response Surface ◽  
Flow Rate ◽  
Mobile Phase ◽  
Hplc Method ◽  
Mobile Phase Flow Rate ◽  
Rp Hplc ◽  
Limit Of Quantitation ◽  
The Impact

In present work, the RP-HPLC method was established for the determination of bromhexine and salbutamol in syrup by using a design of experiment approach. The Plackett-Burman design was applied to screen the influence of independent variables (ratio of organic solvent and pH in mobile phase, flow rate, column temperature, sample injection volume and detection wavelength) on the output data of chromatographic signals (peak area, tailing factor, theoretical plates, resolution) of bromhexine and salbutamol. The Pareto diagram shows that the selected variables affect mainly target function. A central composite design has been used to optimize the values of main factors and Design expert® software predicts the interaction and quadratic model to evaluate the impact of input parameters on output. The optimal conditions were determined with the support of response surface methodology for flow rate 0.9 mL/min, temperature 25 °C and 60% methanol in water with 0.06% orthophosphoric acid as the mobile phase. Good linearity was observed in the concentration range of 8-48 μg/mL for bromhexine and 4-24 μg/mL for salbutamol with a significantly high correlation coefficient (R > 0.999). The limit of detection and limit of quantitation were 0.32 and 0.96 μg/mL, respectively for bromhexine and 0.08 and 0.25 μg/mL, respectively for salbutamol. This method was validated according to ICH guidelines.

SIMULTANEOUS ESTIMATION OF CURCUMIN AND GEFITINIB IN BULK AND TISSUE SAMPLES (PLASMA AND BRAIN HOMOGENATE) BY RP-HPLC: APPLICATION TO A DISTRIBUTION STUDY

INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (07) ◽  
pp. 59-68
Author(s):  
H Mahajan ◽  
S Savale ◽  
P Nerkar ◽  
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Internal Standard ◽  
Brain Homogenate ◽  
Reversed Phase ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Bulk Analysis ◽  
Experimental Conditions ◽  
Rp Hplc

The present study was aimed at developing a Reversed-Phase High-Performance Liquid Chromatography (RP-HPLC) method for simultaneous determination of curcumin (CRM) and gefitinib (GFT) in bulk, plasma and brain homogenate. hydrochlorothiazide was used as an internal standard (IS). A new simple, rapid, selective, precise and accurate RP-HPLC method has been developed. The separation was achieved by using C-18 column (Qualisil BDS C18, 250 mm x 4.6 mm I.D.) coupled with a guard column of silica, mobile phase consisted of acetonitrile: water with 0.1% formic acid (30:70 v/v). The flow rate was 0.2 ml/min and the drug was detected using PDA detector at the wavelength of 242 nm. The experimental conditions, including the diluting solvent, mobile phase composition, column saturation and flow rate, were optimised to provide high-resolution and reproducible peaks. The method was developed and tested for linearity range of 10-60 μg/mL for bulk analysis and 200-800 ng/mL for plasma and brain homogenate. The developed method was validated as per ICH guidelines, in terms of linearity, application of the proposed method to bulk sample, recovery, precision, repeatability, ruggedness, sensitivity (LOD and LOQ) and robustness and stability study (short and long-term stabilities, freeze/thaw stability, post-preparative). The low value of % RSD showed that the method was precise within the acceptance limit of 2%. The developed method was successfully applied for the analysis of the drug in bulk as well as various marketed formulation and drug in plasma and brain distribution studies.

STABILITY-INDICATING RP-HPLC METHOD FOR THE SIMULTANEOUS DETERMINATION OF AMLODIPINE BESYLATE AND AZILSARTAN MEDOXOMIL IN TABLET DOSAGE FORM

INDIAN DRUGS ◽  
2016 ◽  
Vol 53 (06) ◽  
pp. 51-61
Author(s):  
J. G Modi ◽  
◽  
J. K. Patel
Keyword(s):  
Mobile Phase ◽  
Dosage Form ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Good Resolution ◽  
Amlodipine Besylate ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Tablet Dosage ◽  
Azilsartan Medoxomil

A novel, simple, rapid, and highly selective stability indicating RP-HPLC method was developed and validated for simultaneous estimation of azilsartan medoxomil (AZL) and amlodipine besylate HCl (AMLO) in tablet dosage form having strength of 20 mg and 2.5 mg, respectively. The effective chromatographic separation was achieved on a Phenomenex luna ODS C18 (15 cm X 4.6 mm internal diameter, 3.5 μm Particle size) with a mobile phase composed of phosphate buffer (pH-2.5) adjusted with ortho phosphoric acid : acetonitrile in the ratio of 60:40 v/v. The mobile phase was pumped using an isocratic HPLC system at a flow rate of 0.7 mL/min with injection volume 20μl and quantification of the analytes was done at detection wavelength 254 nm. The retention times were found to be 5.918 min and 14.901 min for AMLO and AZL, respectively. The proposed HPLC method was validated with respect to linearity, ranges, precision, accuracy, specificity, robustness, LOD, and LOQ as per ICH Q2 (R1) guideline. Calibration plots were linear over the concentration range of 75-125 µg/mL and 600-1000 µg/mL with correlation coefficients 0.9966 and 0.9948 for AMLO and AZL, respectively. Forced degradation studies were performed using hydrolysis, oxidation, photolytic, and thermal degradation conditions with good resolution between the degradants and analytes. Degradation products resulting from the stress studies did not interfere with the detection of AMLO and AZL, thus the proposed method is sensitive and stability-indicating. The validated HPLC method was successfully applied to the analysis of AMLO and AZL in tablet dosage form.

scholarly journals RP-HPLC method development and validation for simultaneous estimation of Cilnidipine, Atenolol and Chlorthalidone

2018 ◽  
Vol 8 (6-s) ◽  
pp. 78-82 ◽  
Author(s):  
Vishal Singh Solanki ◽  
RAM SINGH BISHNOI ◽  
Raviraj Baghel ◽  
Deepti Jain
Keyword(s):  
High Performance ◽  
Chromatographic Method ◽  
Method Development ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Good Resolution ◽  
Rp Hplc ◽  
Tablet Dosage ◽  
Liquid Chromatographic

A simple precise and economical reverse phase high performance liquid chromatographic method has been developed and validated for the simultaneous estimation of Cilnidipine (CDP), Atenolol (ATL) and Chlorthalidone (CTD).The chromatographic separation was achieved by using Hypersil- keystone C18 (4.6 x 250mm, 5μm) under isocratic conditions The mobile phase consisted of methanol and triple distilled water (80/20, v/v) having pH 7 with a flow rate of 1.0 mL/min. The eluents were monitored at 225 nm for simultaneous measurement.The selected chromatographic conditions were found to effectively separate CDP (Rt: 3.25 min), ATL (Rt: 5.366 min) and CTD (Rt: 9.025 min) having good resolution. The developed method was validated for linearity, accuracy, precision, LOD, LOQ, robustness and for system suitability parameters as per ICH guidelines. In this study, an excellent linearity was obtained with r2 = 0.999, r² = 0.999, r² = 1, for CDP, ATL and CTD respectively. The developed chromatographic method proved to be simple, precise, accurate, robust and reproducible Thus, this method would be employed for routine simultaneous quantification of CDP, ATL and CTD in bulk form or tablet dosage form.   Keywords: Cilnidipine, Atenolol and Chlorthalidone, RP-HPLC.

SIMULTANEOUS DETERMINATION OF DOMPERIDONE AND SOME PRESERVATIVES IN ORAL FORMULATION: RP-HPLC METHOD

INDIAN DRUGS ◽  
2020 ◽  
Vol 57 (05) ◽  
pp. 71-73
Author(s):  
Aasha Patel ◽  
Sandip D. Firke ◽  
Ravindra R. Patil ◽  
Mohan G. Kalaskar ◽  
Sanjay B. Bari ◽  
...  
Keyword(s):  
Flow Rate ◽  
Sodium Benzoate ◽  
Phosphate Buffer ◽  
Gradient Elution ◽  
Oral Formulation ◽  
Hplc Method ◽  
Oral Solution ◽  
Chromatographic Separations ◽  
Rp Hplc

A novel RP-HPLC method was developed and validated for the determination of compounds in an oral solution. The method describes the determination of domperidone along with sodium methylparaben, sodium propylparaben and sodium benzoate in liquid oral formulation. Chromatographic separations were performed using BDS Hypersil 5 μm C18 column and gradient elution (solvent A: phosphate buffer, pH 3.5 and solvent B: methanol), keeping a flow rate of 1.5 mL/min. Detection was done at dual wavelength (232 nm for domperidone and sodium benzoate, and 257 nm for sodium methylparaben and sodium propylparaben). Analysis time was <17 min. The retention times for domperidone, sodium benzoate, sodium methylparaben and sodium propylparaben were found to be 10.0, 6.5, 8.0, and 13.5 min., respectively. The calibration curves for domperidone, sodium benzoate, sodium methylparaben and sodium propylparaben were found to be linear in the range of 250-750, 50-150, 50-150, and 5-15 μg/mL.

RP-HPLC METHOD FOR SIMULTANEOUS ESTIMATION OF METFORMIN HCL AND CANAGLIFLOZIN IN PHARMACEUTICAL FORMULATION

INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (06) ◽  
pp. 49-59
Author(s):  
Hemant Kumar T ◽  
◽  
Gowri Sankar D ◽  
Keyword(s):  
Flow Rate ◽  
Retention Time ◽  
Mobile Phase ◽  
Orthophosphoric Acid ◽  
Hplc Method ◽  
Pharmaceutical Formulation ◽  
Simultaneous Estimation ◽  
Rp Hplc ◽  
Interday Precision ◽  
Metformin Hcl

A simple, specific, accurate, precise and stability-indicating RP-HPLC method was developed and validated for the simultaneous estimation of metformin HCl and canagliflozin in pharmaceutical formulation. The method was developed using the Altima C8 column (150 ×4.6 mm, 0.5 μm) with a mobile phase consisting of acetonitrile and 0.1 % orthophosphoric acid in water (62:38 %V/V) with a flow rate of 1 mL/min. Detection was carried out at 254 nm using a PDA detector. The retention time for metformin HCl and canagliflozin was found to be 2.282 and 3.339 min, respectively. The proposed method was validated for linearity, range, accuracy, precision, robustness, LOD and LOQ. Linearity was observed over a concentration range 15-225 μg/mL for metformin HCl (r2 =0.9995) and 5-40 μg/mL for canagliflozin (r2 =0.9988). The % RSD for intraday and interday precision was found to be 0.13 and 0.20 for metformin HCl and 0.18 and 0.20 for canagliflozin. The LOD and LOQ were found to be 0.16 μg/mL and 0.54 μg/mL for metformin HCl and LOD and LOQ were found to be 0.05 and 0.21 μg/mL for canagliflozin. Metformin HCl and canagliflozin were subjected to stress conditions of degradation including acidic, alkaline, oxidative, thermal and photolysis.

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