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 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.

Analytical method for the determination of curcumin entrapped in polymeric micellar powder using HPLC

2021 ◽  
Vol 32 (4) ◽  
pp. 867-873
Author(s):  
Helmy Yusuf ◽  
Nina Wijiani ◽  
Rizka Arifa Rahmawati ◽  
Riesta Primaharinastiti ◽  
M. Agus Syamsur Rijal ◽  
...  
Keyword(s):  
Flow Rate ◽  
Analytical Method ◽  
Hplc Method ◽  
Array Detector ◽  
Good Resolution ◽  
Diode Array Detector ◽  
Accuracy And Precision ◽  
The Family ◽  
Effective Analysis

Abstract Objectives Curcumin belongs to the family of curcuminoids, natural polyphenolic compounds that possesses neuroprotective properties, anti inflammatory and anticancer. Its entrapment in the developed casein-based micellar powder (CMP) and poloxamer-based micellar powder (PMP) was to enhance the solubility and improve the bioavailability. Henceforth, the present study aimed to acquire an efficient analytical method for the curcumin analysis in polymeric micellar formulations. Methods A fast and specific HPLC method was developed for analyzing curcumin in two different micellar matrices using casein and poloxamer. The HPLC was equipped with a C18 column (250 × 4 mm, 5 µm) and diode array detector. A designated isocratic elution of curcumin was employed using mobile phase with a composition of water (1%, v/v acetic acid) and acetonitrile in a ratio of 50:50 v/v. The employed flow rate was 1.0 mL/min and the analyte was examined at 421 nm. Results An effective analysis in HPLC was successfully achieved by the predetermined HPLC condition. A good resolution of peaks at the employed flow rate was achieved. The linearity was excellent in two different range of concentrations, 2–20 and 10–50 μg/mL. The selectivity, accuracy and precision fulfilled the acceptable requirements. Conclusions The developed method was practically effective to qualitatively identified curcumin. In addition, the assay also effectively quantified the amount of curcumin in the polymeric entrapping matrices which demonstrates that it has great potential to be used in natural compound analysis.

scholarly journals Development of a New HPLC Method for the Simultaneous Determination of Ticarcillin and Clavulanic Acid in Pharmaceutical Formulations

2009 ◽  
Vol 92 (4) ◽  
pp. 1089-1094
Author(s):  
Tai-Li Tsou ◽  
Chiu-Wey Lee ◽  
Hsian-Jenn Wang ◽  
Ya-Chung Cheng ◽  
Yu-Tien Liu ◽  
...  
Keyword(s):  
Clavulanic Acid ◽  
Simultaneous Determination ◽  
Flow Rate ◽  
Ammonium Acetate ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Low Flow ◽  
Hplc Separation ◽  
Accuracy And Precision

Abstract A new HPLC method has been developed and validated for the simultaneous determination of ticarcillin (TIC) and clavulanic acid (CA) in pharmaceutical formulations. The HPLC separation was achieved on a -cyclodextrin column (Cyclobond I, 250 4.6 mm, 5 mm) with methanol16 mM pH 6.0 ammonium acetate buffer (50 + 50, v/v) mobile phase at a flow rate of 0.8 mL/min. Detection was at 220 nm. Validation of the method was performed by evaluating specificity, robustness, accuracy, and precision. The calibration curves were linear in the range of 1100 g/mL for CA and 2200 g/mL for TIC. The LOQs based on the standard regression lines were 0.42 and 1.42 g/mL for CA and TIC, respectively, and the LOD were 0.14 and 0.47 g/mL, respectively. Total recoveries of synthetic mixtures (CA:TIC = 1:10, 1:15, and 1:30) were 99.25100.99 for CA and 99.54100.82 for TIC. Compared with the U.S. Pharmacopeia method, the proposed method has the advantage of a relatively low flow rate and short analysis time. The proposed method was successfully applied for the simultaneous determination of these two drugs in sterilized H2O and 5 dextrose injection solutions.

scholarly journals Development and Validation of HPLC Method for the Simultaneous Determination of Five Food Additives and Caffeine in Soft Drinks

2016 ◽  
Vol 2016 ◽  
pp. 1-8 ◽  
Author(s):  
Bürge Aşçı ◽  
Şule Dinç Zor ◽  
Özlem Aksu Dönmez
Keyword(s):  
Simultaneous Determination ◽  
Flow Rate ◽  
Mobile Phase ◽  
High Performance ◽  
Food Additives ◽  
Hplc Method ◽  
Soft Drinks ◽  
Phase Ratio ◽  
Potassium Sorbate

Box-Behnken design was applied to optimize high performance liquid chromatography (HPLC) conditions for the simultaneous determination of potassium sorbate, sodium benzoate, carmoisine, allura red, ponceau 4R, and caffeine in commercial soft drinks. The experimental variables chosen were pH (6.0–7.0), flow rate (1.0–1.4 mL/min), and mobile phase ratio (85–95% acetate buffer). Resolution values of all peak pairs were used as a response. Stationary phase was Inertsil OctaDecylSilane- (ODS-) 3V reverse phase column (250 × 4.6 mm, 5 μm) dimensions. The detection was performed at 230 nm. Optimal values were found 6.0 pH, 1.0 mL/min flow rate, and 95% mobile phase ratio for the method which was validated by calculating the linearity (r2>0.9962), accuracy (recoveries ≥ 95.75%), precision (intraday variation ≤ 1.923%, interday variation ≤ 1.950%), limits of detection (LODs), and limits of quantification (LOQs) parameters. LODs and LOQs for analytes were in the range of 0.10–0.19 μg/mL and 0.33–0.63 μg/mL, respectively. The proposed method was applied successfully for the simultaneous determination of the mixtures of five food additives and caffeine in soft drinks.

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.

scholarly journals Application of RP-HPLC method for the simultaneous determination of cetirizine in the presence of quinolones

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Hina Shamshad ◽  
Agha Zeeshan Mirza
Keyword(s):  
Human Serum ◽  
Simultaneous Determination ◽  
Flow Rate ◽  
Mobile Phase ◽  
Diclofenac Sodium ◽  
Internal Standard ◽  
Hplc Method ◽  
Rp Hplc ◽  
Ich Guidelines

Abstract Background Present work describes a fast, simple, and sensitive procedure for the simultaneous determination of cetirizine in the presence of quinolones using diclofenac sodium as an internal standard. The present work was designed to analyze these compounds in pharmaceutical and clinical labs being economical for use. Results The mobile phase consisted of the simple composition of methanol, acetonitrile, and water in a ratio of 50:20:30 with a pH adjusted to 3.1 at a flow rate of 1 mL min−1. The UV detection was performed at 225 nm. The linearity was assessed over the range of 2.5–50 μg mL−1 for all drugs. The parameters such as accuracy, precision, linearity (>0.999), and sensitivity were satisfactory. Conclusion The method was equally applicable for formulation and human serum with recovery values between 95 and 105%. The results of the method were validated statistically according to ICH guidelines.

scholarly journals HPLC method development for determination of metoprolol, telmisartan and cilnidipine simultaneously using response surface design

2021 ◽  
Vol 12 (1) ◽  
pp. 602-610
Author(s):  
Jayaseelan S ◽  
Kannappan N ◽  
Ganesan V
Keyword(s):  
Quantitative Methods ◽  
Method Development ◽  
Desirability Function ◽  
Cost Effective ◽  
Drug Dosage ◽  
Hplc Method ◽  
Good Resolution ◽  
Simple Method ◽  
Short Run

The development of an HPLC method for determination of Metoprolol, Telmisartan and Cilnidipine simultaneously in additional dosage was not published or reported up till date. The main aim of our study was to design a simultaneous and multiple response optimizations using the Derringer's desirability function in order to estimate Metoprolol, Telmisartan and Cilnidipine in pharmaceutical and bulk drug dosage form by HPLC method with experiment central compositive design (CCD) protocol for the quantitative methods analysis and also for validation of the procedure that is developed as per ICH regulations. An innovative RP-HPLC method had been designed for the estimation of Metoprolol, Telmisartan and Cilnidipine simultaneously in formulation using central composite design. Three factors were investigated and determined as significant when compared to the interaction and quadratic effect of the samples that CCD along with the response of the surface methodology. The developed method produced a good resolution of the drugs with a very short run time of 7.5 min. It was also validated according to ICH guidelines. It was recognized as novel and simple method that is accurate and cost-effective. So the proposed method fits best in the assaying routine of Metoprolol, Telmisartan and Cilnidipine in any formulations produced by quality control laboratories.

STABILITY INDICATING RP-HPLC METHOD FOR SIMULTANEOUS DETERMINATION OF CEFTRIAXONE SODIUM AND SALBUTAMOL

INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (09) ◽  
pp. 65-69
Author(s):  
Atul Sherje ◽  
◽  
Subhash Dhende ◽  
Mayur Yergiri
Keyword(s):  
Simultaneous Determination ◽  
Chromatographic Method ◽  
Hplc Method ◽  
Good Resolution ◽  
Ceftriaxone Sodium ◽  
Ich Guidelines ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic ◽  
Potassium Dihydrogen Orthophosphate

An isocratic liquid chromatographic method with UV detection at 230 nm is described for simultaneous determination of ceftriaxone sodium and salbutamol in bulk. Chromatographic separation of the two drugs was achieved on an Inertsil ODS© C18 (250 × 4.6 mm, 5 μ) using a mobile phase consisting of 50 mM potassium dihydrogen orthophosphate and methanol (77:23 %V/V) adjusted to pH 7.0 with triethylamine at a fl ow rate of 1.0mL min-1. The optimum separation was achieved in less than 10 minutes. The developed liquid chromatographic method offers symmetric peak shape, good resolution and reasonable retention time for both drugs. The method was validated as per ICH guidelines.

Development and Validation of an HPLC Method for the Simultaneous Determination of Fipronil, Chlorfenapyr, and Pyriproxyfen in Insecticide Formulations

2016 ◽  
Vol 99 (5) ◽  
pp. 1185-1190 ◽  
Author(s):  
Anum Hafeez ◽  
Iffat Abdul Tawab ◽  
Sajid Iqbal
Keyword(s):  
Simultaneous Determination ◽  
Method Development ◽  
Low Cost ◽  
Hplc Method ◽  
Good Resolution ◽  
Chromatographic Separations ◽  
Method Development And Validation ◽  
Development And Validation ◽  
Interday Precision

Abstract In this study, the analytical method development and validation of an HPLC assay for simultaneous determination of fipronil, chlorfenapyr, and pyriproxyfen in formulation products is described. On the basis of solubility and chromatographic separation with good resolution, acetonitrile–water (80 + 20) was selected as the mobile phase in isocratic mode with a flow rate of 1 mL/min. Chromatographic separations were performed on a Beckman C18 analytical column (4.6 mm × 15 cm, 5 μm particle size; Musa Jee & Sons, Karachi, Pakistan). The retention times for fipronil, chlorfenapyr, and pyriproxyfen were 3.70, 8.61 and 10.09 min, respectively. Calibration curves of all studied insecticides were linear in the concentration range of 20 to 800 μg/mL, with R2 &gt; 0.997. The LODs of fipronil, chlorfenapyr, and pyriproxyfen were 15.1, 13.3, and 20.0 μg/mL, respectively, whereas the LOQs were 45.9, 40.3, and 60.6 μg/mL. Interday precision was RSD, % &lt;2 for all formulation types, whereas intraday precision was &lt;3. The accuracy of the proposed method was determined by interlaboratory comparison. The z-score for all formulation results were &lt;2.The proposed method is low-cost, green, accurate, and precise and can suitably be used for the simultaneous quantitative determination of fipronil, chlorfenapyr, and pyriproxyfen in their formulations.

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