Multivariate Optimization of Separation Conditions for Simultaneous Determination of Acemetacin and Chlorzoxazone in a Pharmaceutical Preparation by HPLC Using Response Surface Methodology

2013 ◽  
Vol 96 (4) ◽  
pp. 723-729
Author(s):  
Cigdem Aybaba ◽  
Ismail Murat Palabiyik ◽  
Mehmet Gokhan Caglayan ◽  
Feyyaz Onur
Keyword(s):  
Response Surface Methodology ◽  
Response Surface ◽  
Simultaneous Determination ◽  
Mobile Phase ◽  
Ammonium Acetate ◽  
Pharmaceutical Preparation ◽  
Internal Standard ◽  
Hplc Method ◽  
Optimum Separation

Abstract A new, fast, accurate, precise, and sensitive RP-HPLC method for the simultaneous determination of acemetacin and chlorzoxazone has been developed. Response surface methodology with a central composite design was used to optimize the acetonitrile and ammonium acetate percentage in the mobile phase and pH of ammonium acetate. The optimum separation was achieved on a C18 column (250 × 4.6 mm id, 5 μm particle size) using the mobile phase methanol–acetonitrile–0.02 M ammonium acetate, pH 9.4 (25 + 35 + 40, v/v/v) at a flow rate of 1.5 mL/min; UV detection at 270 nm, and cyanocobalamin as an internal standard. This developed method was validated and successfully applied to a coated tablet pharmaceutical preparation.

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 Optimization and Validation of an RP-HPLC Method for Analysis of Hydrocortisone Acetate and Lidocaine in Suppositories

2010 ◽  
Vol 93 (1) ◽  
pp. 102-107 ◽  
Author(s):  
Biljana Jancic-Stojanović ◽  
Andjelija Malenović ◽  
Slavko Marković ◽  
Darko Ivanović ◽  
Mirjana Medenica
Keyword(s):  
Particle Size ◽  
Response Surface Methodology ◽  
Mobile Phase ◽  
Orthophosphoric Acid ◽  
Internal Standard ◽  
Hplc Method ◽  
Hydrocortisone Acetate ◽  
Rp Hplc ◽  
Method Optimization

Abstract An RP-HPLC method has been optimized and validated for the simultaneous determination of hydrocortisone acetate and of lidocaine in suppositories. For the method optimization, response surface methodology was applied, and the obtained model was tested using analysis of variance. The optimal separations were conducted on a Beckman-Coulter 150 4.6 mm, 5 µm particle-size column at 20C. The mobile phase was methanolwater (65 + 35, v/v), pH adjusted to 2.5 with 85% orthophosphoric acid, with a flow rate of 1.0 mL/min. UV detection was performed at 250 nm. Phenobarbital was used as an internal standard. The method was validated for selectivity, linearity, precision, and robustness.

scholarly journals Application of Response Surface Methodology in Development and Optimization of Stability Indicating RP-HPLC Method for Determination of Tolvaptan in Bulk and Formulation

2021 ◽  
pp. 137-148
Author(s):  
A. S. Sutar ◽  
C. S. Magdum
Keyword(s):  
Response Surface Methodology ◽  
Response Surface ◽  
Design Of Experiment ◽  
Mobile Phase ◽  
Method Development ◽  
Degradation Products ◽  
Hplc Method ◽  
Stability Indicating ◽  
Rp Hplc

Design of Experiment assisted stability indicating RP-HPLC was developed and optimized using response surface methodology for determination of Tolvaptan.  Mobile phase was developed and optimized using Design of Experiment with response surface methodology. Acetonitrile and phosphate buffer with pH 5.5 (70:30% V/V) was optimized as mobile phase. The flow rate was maintained at 1ml/min. Stress studies were performed as per guidelines. Method was validated in accordance with regulatory requirements and results were within specified limits of regulatory guidelines. Tolvaptan was eluted at 3.24 min. It shows linearity from 2.5-15 µg/ml. Coefficient of correlation was 0.999, LOD and LOQ values were 1.0871 (µg/ml) and 3.2942 (µg/ml). Precision was determined with % RSD of 0.8669 and 0.9709%, mean percentage Recovery value was found to be 99.88 ±1.2. All stress degradation products are very well resolved from drug peak which indicate suitability indicating nature of the developed method. Design of Experiment technique can help in fast and economical optimization of mobile phase which inturn will save time for method development. The developed method is simple, accurate, sensitive which can be utilised as stability indicating method for identification of degradation products in routine analysis of the drug.

scholarly journals DEVELOPMENT AND VALIDATION OF A HPLC METHOD FOR THE SIMULTANEOUS DETERMINATION OF PSEUDOEPHEDRINE, DEXTROMETHORPHAN, AND TRIPROLIDINE IN THEIR COMBINED COUGH AND COLD SYRUPS

2017 ◽  
Vol 13 (11) ◽  
pp. 6011-6017
Author(s):  
Imad Osman Abu Reid ◽  
Elrasheed Ahmed Gad Kariem
Keyword(s):  
Simultaneous Determination ◽  
Mobile Phase ◽  
Pharmaceutical Preparation ◽  
Hplc Method ◽  
Intermediate Precision ◽  
Cation Exchange Column ◽  
Method Accuracy ◽  
Development And Validation ◽  
Liquid Chromatographic

A simple and efficient liquid chromatographic method has been developed and validated for the simultaneous determination of pseudoephedrine, dextromethorphan, and triprolidine in cough and cold syrup. The separation of the analytes was achieved within 10min, employing a mixture of 50% v/v methanol-water containing 35.07 mM/L ammonium acetate adjusted to pH 5.58 as isocratic mobile phase, pumped at 1.0 ml min-1 through a strong cation exchange column (10µm particle size). The analytes were detected at 265nm. Statistical experimental designs and graphic representations (response surface methodologies, Pareto charts) were used for optimizing the mobile phase composition. The linearity of the calibration (r>0.99, n =18) in the relevant ranges (up to 125% of the expected concentrations of the analytes in the formulation), method accuracy (RSD <2.0%), repeatability (RSD<2.0%) and intermediate precision, were verified. System suitability parameters were also determined. The validated method was successfully employed for the routine analysis of a syrup pharmaceutical preparation against cough and cold, showing satisfactory analytes recoveries and precsion.

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 Determination of Chloroquine and Pyrimethamine with Cetirizine in an Active Form and Human Serum by RP-HPLC

2021 ◽  
Author(s):  
Hina Shamshad ◽  
Ali Sayqal ◽  
Jahan Zeb ◽  
Agha Zeeshan Mirza
Keyword(s):  
Human Serum ◽  
Simultaneous Determination ◽  
Active Form ◽  
Internal Standard ◽  
Hplc Method ◽  
Serum Samples ◽  
Rp Hplc ◽  
Cetirizine Hydrochloride ◽  
Bulk Drug

Abstract A simple, accurate and precise RP-HPLC method was developed for the simultaneous determination of chloroquine, pyrimethamine and cetirizine hydrochloride concentrations in bulk drug and human serum. The assay was performed using a mobile phase of methanol: water (70:30) at pH of 2.8 ± 0.05 on the Purospher C-18 column with UV detection at 230 nm and rosuvastatin used as an internal standard. The retention times observed for chloroquine, pyrimethamine and cetirizine hydrochloride were 3.5, 2.5 and 5.5 minutes, respectively. The method was found to be specific for the assayed drugs showing a linear response in the concentration range of 1–100 μg mL−1 with coefficients of determination values of (r = 0.999). The method was developed and validated according to ICH guidelines. The method was used to monitor the serum samples and was found to be sensitive for therapeutic purposes, showing the potential to be a useful tool for routine analysis in laboratories.

scholarly journals Simultaneous Determination of Preservatives (Methyl Paraben and Propyl Paraben) in Sucralfate Suspension Using High Performance Liquid Chromatography

2011 ◽  
Vol 8 (1) ◽  
pp. 340-346 ◽  
Author(s):  
Rajesh M. Kashid ◽  
Santosh G. Singh ◽  
Shrawan Singh
Keyword(s):  
High Performance Liquid Chromatography ◽  
Simultaneous Determination ◽  
Mobile Phase ◽  
High Performance ◽  
Reversed Phase ◽  
Hplc Method ◽  
Reversed Phase Hplc ◽  
Methyl Paraben ◽  
Propyl Paraben

A reversed phase HPLC method that allows the separation and simultaneous determination of the preservatives methyl paraben (M.P.) and propyl paraben (P.P.) is described. The separations were effected by using an initial mobile phase of water: acetonitrile (50:50) on Inertsil C18 to elute P.P. and M.P. The detector wavelength was set at 205 nm. Under these conditions, separation of the two components was achieved in less than 10 min. Analytical characteristics of the separation such as precision, specificity, linear range and reproducibility were evaluated. The developed method was applied for the determination of preservative M.P. and P.P. at concentration of 0.01 mg/mL and 0.1 mg/mL respectively. The method was successfully used for determining both compounds in sucralfate suspension.

Simultaneous determination of Sulphadoxine and Pyrimethamine by taking Tolterodine as an internal standard in Pharmaceutical dosage form by RP-HPLC

2021 ◽  
pp. 145-150
Author(s):  
Sushil D. Patil ◽  
Pravin B. Shelke ◽  
Priti Aher ◽  
Maswood Ahmed Hafizur Rahman
Keyword(s):  
Simultaneous Determination ◽  
Dosage Form ◽  
Internal Standard ◽  
Hplc Method ◽  
Control Analysis ◽  
Pharmaceutical Dosage Form ◽  
Quality Control Analysis ◽  
Rp Hplc ◽  
Sulphadoxine Pyrimethamine

A simple, rapid, economic, sensitive and precise HPLC method has been developed for the simultaneous determination of Sulphadoxine and Pyrimethamine in pharmaceutical dosage form by taking Tolterodine as an internal standard. The method was carried out using Phenomenex C18 (4.6ID × 250mm; 5µm) column and mobile phase comprised of methanol and Phosphate Buffer in proportion of ratio 60:40 v/v. The flow rate was 1.0mL/min and detection was carried out at 276nm. The retention time of Sulphadoxine, Pyrimethamine and Tolterodine were found to be 2.967, 4.058 and 6.908 respectively. Linearity of Sulphadoxine and Pyrimethamine in the range of 2 to 12μg/mL and 4 to 24μg/mL respectively. The % recoveries of Sulphadoxine and Pyrimethamine were found to be in between 99.93% to 99. 96 % respectively. The proposed method is suitable for the routine quality control analysis for simultaneous determination of Sulphadoxine and Pyrimethamine was in bulk and pharmaceutical dosage form.

scholarly journals Rapid Determination of α-Hederin and Hederacoside C in Extracts of Hedera helix Leaves Available in the Czech Republic and Poland

2015 ◽  
Vol 10 (9) ◽  
pp. 1934578X1501000
Author(s):  
Lucie Havlíková ◽  
Kateřina Macáková ◽  
Lubomír Opletal ◽  
Petr Solich
Keyword(s):  
Mobile Phase ◽  
Ammonium Acetate ◽  
Rapid Determination ◽  
Hplc Method ◽  
Leaf Extracts ◽  
Hedera Helix ◽  
The Czech Republic ◽  
Upper Respiratory ◽  
Isocratic Mode

Leaf extracts of Hedera helix L. are widely used in the treatment of upper respiratory diseases. The saponins α-hederin and hederacoside C are considered to be the main compounds responsible for the biological activity. α-Hederin and hederacoside C were determined in H. helix leaf extracts using a fast, simple and validated HPLC method. An XTerra MS C18 column and mobile phase composed of 10 mM ammonium acetate at pH 8.5 (adjusted with triethylamine) and acetonitrile were used for the chromatography at 1.2 mL min−1. The column was kept at 30°C. Detection was performed at 220 nm. An approach utilizing a basic pH of the aqueous part of the mobile phase enabled analysis in 5 minutes in isocratic mode. The method was validated and used for the quality control of H. helix leaf ethanolic extracts.

scholarly journals Development of a Method to Determine Albendazole and Its Metabolites in the Muscle Tissue of Yellow Perch Using High-Performance Liquid Chromatography with Fluorescence Detection

2011 ◽  
Vol 94 (2) ◽  
pp. 446-452 ◽  
Author(s):  
Donglei Yu ◽  
Nathan Rummel ◽  
Badar Shaikh
Keyword(s):  
High Performance Liquid Chromatography ◽  
Muscle Tissue ◽  
Mobile Phase ◽  
Yellow Perch ◽  
High Performance ◽  
Ammonium Acetate ◽  
Hplc Method ◽  
Tissue Samples ◽  
Phase Combination

Abstract An HPLC method was developed for the determination of albendazole (ABZ) and its metabolites, a sulfoxide (ABZSO), a sulfone (ABZSO2), and albendazole-2-aminosulfone (ABZ-2-NH2SO2), from yellow perch muscle tissue with adhering skin. The muscle tissue samples were made alkaline with potassium carbonate and extracted with ethyl acetate, followed by a series of liquidliquid extraction steps. After solvent evaporation, the residue was reconstituted in the initial mobile phase combination of the gradient. The mobile phase consisted of a buffer, 50 mM ammonium acetate (pH 4.0) in 10 methanolwater, and 100 acetonitrile. The gradient was from 20 acetonitrile to 85 acetonitrile. The analytes were chromatographed on an RP Luna C18(2) column and detected by fluorescence with excitation and emission wavelengths of 290 and 330 nm, respectively. The average recoveries from fortified muscle tissue for ABZ (20100 ppb), ABZ-SO (20200 ppb), ABZSO2 (8100 ppb), and ABZ-2-NH2SO2 (20100 ppb) were 85, 95, 101, and 86, respectively, with corresponding CV values of 9, 3, 6, and 4, respectively. Their LOQ values were 10, 10, 1, and 10 ppb, respectively. The procedure was applied to determine ABZ and its major metabolites in the incurred muscle tissue of yellow perch obtained after orally dosing the fish with ABZ.

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