OPTIMIZATION OF RP-HPLC METHOD BY 32 – CENTRAL COMPOSITE DESIGN FOR THE VALIDATION AND ESTIMATION OF DOXYCYCLINE HYCLATE IN BULK DRUG AND FORMULATIONS

INDIAN DRUGS ◽  
2015 ◽  
Vol 52 (11) ◽  
pp. 42-49
Author(s):  
C Dhal ◽  
◽  
F. J. Ahmad ◽  
M. Singhal ◽  
A. Kukrety ◽  
...  
Keyword(s):  
Central Composite Design ◽  
Flow Rate ◽  
High Performance ◽  
Hplc Method ◽  
Array Detector ◽  
Doxycycline Hyclate ◽  
Chromatography Method ◽  
Column Temperature ◽  
Bulk Drug ◽  
Central Composite

An accurate, sensitive, precise, economic and rapid isocratic Reverse Phase High Performance Liquid Chromatography method was developed complying Quality by Design (QbD) trends and validated for determining doxycycline hyclate in bulk drug, tablet and capsule dosage form. The method was optimized using Minitab software with 3 factors (pH of the buffer, flow rate and percentage of buffer in the mobile phase), 2 level (higher limit and lower limit) Central Composite Design (CCD). The results of randomized 20 runs were analyzed for optimum composite desirability to give optimum conditions such as, pH 6.5, flow rate 0.9 mLmin-1 and 30:70 V/V 0.05M potassium dihydrogen orthophosphate buffer adjusted to pH 6.5 using orthophosphoric acid and methanol using C8 column 250 X 4.6 mm X 5.0 μm, injection volume of 10uL, ambient column temperature and ultraviolet detection using photo diode array detector at 360nm as constants. The method was validated as per ICH guidelines and was found linear over a concentration range of 10-100 μg/mL (r2 = 0.999) with the limits of detection and quantification being 2.45 μg/mL and 7.55 μg/mL respectively.

scholarly journals Optimization of HPLC Using Central Composite Design for Determination of Curcumin and Demethoxycurcumin in Tablet Dosage Form

2018 ◽  
Vol 16 (2) ◽  
pp. 137-145
Author(s):  
Chairany Siregar ◽  
Niken K Prabaningdyah ◽  
Syaiful Choiri ◽  
Sugeng Riyanto ◽  
Abdul Rohman
Keyword(s):  
Acetic Acid ◽  
Central Composite Design ◽  
High Performance ◽  
Effective Means ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Column Temperature ◽  
Validation Parameters ◽  
Tablet Dosage ◽  
Central Composite

In this study, central composite design (CCD) was used for optimization of high performance liquid chromatographic (HPLC) method for simultaneous analysis of curcumin (CUR) and demethoxycurcumin (DMC) in tablets containing Curcuma extract. Separation of CUR and DMC was performed using X-Bridge C18 column (250 x 4.6 mm i.d; 5 μm). Four factors that were investigated include the concentration of acetic acid (X1), ratio of acetic acid (X2), flow rate of mobile phase (X3) and column temperature (X4). Based on responses obtained (retention time, peak area, resolution and tailing factor), the optimum condition selected was X1 = 3.00%, X2 = 51%, X3 = 1.05 mL/min and X4 = 45oC. This HPLC condition was validated by assessing several validation parameters including system suitability test, selectivity, linearity, precision, accuracy and robustness according to International Conference Harmonization (ICH). All validation parameters meet the acceptance criteria set by ICH. The validated method was successfully used for analysis of CUR and DMC in tablets containing Curcuma extract. CCD was effective means in optimization of HPLC for analysis of CUR and DMC in pharmaceutical formulation.Dhaka Univ. J. Pharm. Sci. 16(2): 137-145, 2017 (December)

RP-HPLC Method for Determination of Gemfibrozil using Central Composite Design (CCD)

2021 ◽  
pp. 3009-3014
Author(s):  
Ajay I. Patel ◽  
Krupa B. Prajapati ◽  
Swati H. Jolapara ◽  
Amitkumar J. Vyas ◽  
Ashok B. Patel ◽  
...  
Keyword(s):  
Central Composite Design ◽  
Flow Rate ◽  
High Performance ◽  
Dosage Form ◽  
Hplc Method ◽  
Rp Hplc ◽  
Central Composite ◽  
Theoretical Plates ◽  
Analytical Liquid Chromatography

The high-Performance Analytical Liquid Chromatography (HPLC) method (AQbD) for routine analysis of Gemfibrozil in dosage form was developed in column C18 using an experimental design. The central composite design (CCD) was adopted in evaluating the responses and robustness of the method. In the project, the combined effect of buffer pH, % organic phase and flow rate, each at five levels, was selected for responses such as retention time and number of theoretical plates, then interpreted and optimized statistically with the help of the surface methodology of response and therefore of the analysis of the constructed models and of the outline graphs was obtained. Acetonitrile: phosphate buffer (pH-4) (59: 41% v / v) as eluent at a flow rate of 1.0ml/min was found to be the optimal condition for obtaining the desired answers.

scholarly journals Gradient High Performance Liquid Chromatography method for determination of related substances in (7-{4-[4-(1-Benzothiophen-4-YL] Butoxy} Quinolin-2(1H)-one) dosage form

2019 ◽  
Vol 9 (1-s) ◽  
pp. 36-43
Author(s):  
B. Karuna Kumar ◽  
K.B Chandra Shekar ◽  
V. Guna Sekaran
Keyword(s):  
Flow Rate ◽  
High Performance ◽  
Drug Product ◽  
Wave Length ◽  
Hplc Method ◽  
Chromatography Method ◽  
Column Temperature ◽  
Stability Indicating ◽  
Related Substances ◽  
Stability Indicating Method

A sensitive HPLC method was developed and validated for the estimation of related substances in Brexpiprazole in drug Product. The developed method is found to be specific, reproducible, and stability indicating. Kromasil100-5 C18 (150x4.6mm), 5μ column was used and mobile phase consisted of mixture of phosphate buffer of pH5.2 and ACN in gradient program is used at a flow rate of 1.0mL/min at a wave length of 215 nm. The detector linearity was established from concentrations ranging from LOQ-150% of specification level with a correlation co-efficient of 0.999. The method was also validated for specificity, LOD, LOQ, accuracy, robustness, precision. The method is proved to be robust with respect to change in flow rate, pH, organic phase composition and column temperature. The proposed method is found to be sensitive, precise, rapid, reproducible, and offers good column life. Keywords: RP-HPLC; Stability indicating method; Brexpiprazole; validation.

DEVELOPMENT AND VALIDATION OF RP-HPLC METHOD FOR THE DETERMINATION OF ZOLMITRIPTAN IN BULK DRUG AND TABLET DOSAGE FORM

INDIAN DRUGS ◽  
2013 ◽  
Vol 50 (08) ◽  
pp. 20-26
Author(s):  
P. K Arora ◽  
◽  
A. Chauhan ◽  
D Duggal ◽  
P. K., Saini ◽  
...  
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
Hplc Method ◽  
Array Detector ◽  
Calibration Plot ◽  
Chromatography Method ◽  
Liquid Chromatography Method ◽  
Elution Method ◽  
Bulk Drug ◽  
Tablet Dosage

A convenient, simple, accurate, precise and reproducible Reverse Phase High Performance Liquid Chromatography method was developed and validated for the estimation of zolmitriptan in the bulk drug and tablet dosage form. Objective was achieved under optimized chromatographic conditions on Dionex UHPLC system with Dionex C18 column (250 × 4.6 mm, 5 mcm particle size) using mobile phase composed of methanol and 0.005 M ammonium acetate in the ratio of 50:50 V/V. The separation was achieved using an isocratic elution method with a flow rate of 1 mL/ min at room temperature. The effluent was monitored at 230 nm using diode array detector. The retention time of zolmitriptan was found to be 3.4 minutes and the standard calibration plot was linear over a concentration range of 10–120 mcg/ mL with r2 = 0.9999. The LOD and the LOQ were found to be 3.7 mcg/ mL and 11.1 mcg/ mL respectively. The amount of zolmitriptan present in the bulk drug was 99.81 % and in the formulation 98.05 % of the stated amount respectively. The method was validated statistically using the %RSD and the values are found to be within the limits. The recovery studies were performed and the percentage recoveries were found to be 99.2± 0.5706 %. So, the proposed method was found to be simple, specific, linear, and robust. Hence this method was conveniently and easily applied for routine analysis of zolmitriptan in bulk drug and tablet dosage form.

scholarly journals Development and validation of RP-HPLC method for estimation of brexpiprazole in its bulk and tablet dosage form using Quality by Design approach

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Amol S. Jagdale ◽  
Nilesh S. Pendbhaje ◽  
Rupali V. Nirmal ◽  
Poonam M. Bachhav ◽  
Dayandeo B. Sumbre
Keyword(s):  
Flow Rate ◽  
High Performance ◽  
Reversed Phase ◽  
Hplc Method ◽  
Control Analysis ◽  
Uv Detector ◽  
Mobile Phase Flow Rate ◽  
Rp Hplc ◽  
Quality By Design Approach ◽  
Bulk Drug

Abstract Background A new, sensitive, suitable, clear, accurate, and robust reversed-phase high-performance liquid chromatography (RP-HPLC) method for the determination of brexpiprazole in bulk drug and tablet formulation was developed and validated in this research. Surface methodology was used to optimize the data, with a three-level Box-Behnken design. Methanol concentration in the mobile phase, flow rate, and pH were chosen as the three variables. The separation was performed using an HPLC method with a UV detector and Openlab EZchrom program, as well as a Water spherisorb C18 column (100 mm × 4.6; 5m). Acetonitrile was pumped at a flow rate of 1.0 mL/min with a 10 mM phosphate buffer balanced to a pH of 2.50.05 by diluted OPA (65:35% v/v) and detected at 216 nm. Result The developed RP-HPLC method yielded a suitable retention time for brexpiprazole of 4.22 min, which was optimized using the Design Expert-12 software. The linearity of the established method was verified with a correlation coefficient (r2) of 0.999 over the concentration range of 5.05–75.75 g/mL. For API and formulation, the percent assay was 99.46% and 100.91%, respectively. The percentage RSD for the method’s precision was found to be less than 2.0%. The percentage recoveries were discovered to be between 99.38 and 101.07%. 0.64 μg/mL and 1.95 μg/mL were found to be the LOD and LOQ, respectively. Conclusion The developed and validated RP-HPLC system takes less time and can be used in the industry for routine quality control/analysis of bulk drug and marketed brexpiprazole products. Graphical abstract

VALIDATED RP-HPLC METHOD FOR DETERMINATION OF ENZALUTAMIDE IN BULK DRUG AND PHARMACEUTICAL DOSAGE FORM

INDIAN DRUGS ◽  
2016 ◽  
Vol 53 (11) ◽  
pp. 46-50
Author(s):  
Z. G Khan ◽  
◽  
S. S. Patil ◽  
P. K. Deshmukh ◽  
P. O. Patil
Keyword(s):  
Retention Time ◽  
Mobile Phase ◽  
High Performance ◽  
Reversed Phase ◽  
Hplc Method ◽  
Uv Detector ◽  
Chromatography Method ◽  
Pharmaceutical Dosage Form ◽  
Bulk Drug

Novel, isocratic reversed phase high performance liquid chromatography method was developed and validated for the determination of enzalutamide (EZA) in bulk drug and pharmaceutical formulation. Efficient separation was achieved on PrincetonSPHER C18 100A, 5μ (250×4.6 mm) under the isocratic mode of elution using acetonitrile: water (80:20) % V/V as a mobile phase pumped in to the column at flow rate 1.0 mL/min. The effluent was monitored at 237.0 nm using UV detector. EZA was eluted in the given mobile phase at retention time (tR) of 3.2 minutes. The standard calibration curve was linear over the concentration range 10 - 60 μg/mL with correlation coefficient 0.997. The method was validated for accuracy, precision, sensitivity, robustness, ruggedness and all the resulting data treated statistically. The system suitability parameters like retention time, theoretical plates, tailing factor, capacity factor were found within the limit.

scholarly journals DEVELOPMENT OF A HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR ANALYZING DISODIUM 5′-GUANYLATE AND DISODIUM 5′-INOSINATE LEVELS IN FLAVOR ENHANCERS

2018 ◽  
Vol 10 (1) ◽  
pp. 133
Author(s):  
Dwi Karina Natalia ◽  
Harmita . ◽  
Taufiq Indra Rukmana
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Flow Rate ◽  
Phosphate Buffer ◽  
Mobile Phase ◽  
High Performance ◽  
Potassium Phosphate ◽  
Array Detector ◽  
Potassium Phosphate Buffer ◽  
Chromatography Method

Objective: This study aimed to develop a selective analytical method for assessing disodium 5′-guanylate and disodium 5′-inosinate levels in flavorenhancers.Methods: The levels were assessed using high-performance liquid chromatography (HPLC) with a photodiode array detector (PDA) (wavelength=255 nm) and a SunFire® C18 column (250 mm × 4.6 mm × 5 μm). The mobile phase comprised a mixture of potassium phosphate buffer and anion pair reagent-hexane-1-sulfonic acid sodium salt - with a flow rate of 1.2 mL/min. The ion pair was used to generate a neutral equilibrium, whichresulted in increased retention of the analytes. Optimized analysis conditions were then validated regarding accuracy, precision, linearity, selectivity,and the limits of detection and quantification.Results: The average levels of disodium 5′-inosinate in the six analyzed samples were 0.24±1.46, 0.21±2.69, 0.58±3.26, 0.21±0.84, 0.22±3.59, and0.47±2.21%, respectively. Regarding disodium 5′-guanylate, the average levels were 0.15±2.85, 0.15±0.12, 0.41±3.80, 0.16±1.72, 0.27±1.18, and0.34±1.83, respectively.Conclusion: The optimal conditions for analyzing disodium 5′-guanylate and disodium 5′-inosinateusing HPLC with a PDA and SunFire C18 columnwere λ=255 nm, a mobile phase of potassium phosphate buffer and sodium hexane sulfonate, and a flow rate of 1.2 mL/min. For disodium 5′-inosinate,its average levels in samples A–F were 0.24±1.46, 0.21±2.69, 0.58±3.26, 0.21±0.84, 0.22±3.59, and 0.47±2.21%, respectively. Meanwhile, the averagelevels of disodium 5′-guanylate in the samples were 0.15±2.85, 0.15±0.12, 0.41±3.80, 0.16±1.72, 0.27±1.18, and 0.34±1.83%, respectively.

scholarly journals THE OPTIMIZATION OF HPLC FOR QUANTITATIVE ANALYSIS OF ACID ORANGE 7 AND SUDAN II IN COSMETIC PRODUCTS USING BOX BEHNKEN DESIGN

2019 ◽  
pp. 130-137 ◽  
Author(s):  
NOVALINA BR PURBA ◽  
ABDUL ROHMAN ◽  
SUDIBYO MARTONO
Keyword(s):  
Flow Rate ◽  
Retention Time ◽  
Mobile Phase ◽  
High Performance ◽  
Hplc Method ◽  
Acid Orange 7 ◽  
Column Temperature ◽  
Box Behnken Design ◽  
Acid Orange

Objective: The objective of this study was to optimize high-performance liquid chromatography (HPLC) method for the determination of acid orange 7 (AO7) and sudan II (SII) in blusher product based on response surface methodology using box behnken design (BBD) approach. Methods: Some factors responsible for HPLC separation including column temperature, mobile phase composition, flow rate were optimized using BBD. The responses evaluated were peak area, retention time, and tailing factor. AO7 and SII in blusher product has different properties, therefore both analytes were analysed using C18 column (Thermo Synergy Gold 250 mm x 4.6 mm i.d.,5 µm) using Shimadzu LC 20AD chromatograph equipped with photo-diode array (PDA) detector at 300-650 nm. The mobile phase used was acetonitrile-water (1:1 v/v), and acetonitrile composition was optimized at 35-50% for separation AO7 (ACN1), and 80-90% for SII (ACN2), delivered at the flow rate of 0.9–1 ml/min, using column temperature at 30-40 °C. Results: BBD showed that separation of AO7 was influenced by the concentration of ACN1, flow rate and column temperature. These factors affected retention time, peak area, and tailing factor with peak area was the most significant. Tailing factor was not significantly affected by each factor, and retention time was slightly effected. Otherwise, Sudan II was affected by all these factors except ACN1. The optimal condition obtained based BBD was ACN1 43%, ACN2 90%, the flow rate of 0.9 ml/min and a column temperature of 40 °C. Conclusion: BBD can be used to get optimum condition for analysis of AO7 and SII in blusher product.

scholarly journals HPLC method validation for quantification of tetrahydrocurcumin in bulk drug and formulation

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Roopam Raut ◽  
Jessy Shaji
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Wide Spectrum ◽  
Cost Effective ◽  
Hplc Method ◽  
Uv Detector ◽  
Column Temperature ◽  
Ich Guidelines ◽  
Recovery Study ◽  
Bulk Drug

Abstract Background Tetrahydrocurcumin (THC), the active metabolite of curcumin, is gaining popularity amongst scientist due to its wide spectrum of pharmacological activities, better stability and colourless nature. The objective of this study was to develop a sensitive, cost-effective RP-HPLC method for the estimation of THC in bulk drug substance and formulation. Results Efficient chromatographic separation was achieved on Hypersil BDS, C18 column, 250 mm × 4.6 mm, 5 μm column by isocratic elution with mobile phase comprising of acetonitrile: methanol: water (40:23:37% V/V); adjusted to a pH of 3.0 ± 0.05. The flow rate of the mobile phase was 1.0 ml/min with a column temperature of 25 °C. UV detector was used for the analysis and detection was carried out at 280 nm. The developed method was validated according to ICH guidelines with respect to system suitability, linearity, accuracy, precision and robustness. The theoretical plates were found to be more than 5800. The method showed linearity over the range of 4 to 60 μg/ml with R2 = 0.9998. The accuracy of the method in terms of recovery study was 98.23-99.99%. The %RSD for intra-day and inter-day precision were 0.272 and 0.275, respectively. The method was found to be robust with respect to change in wavelength, flow rate and column temperature. Conclusion The analytical method was found satisfactory on validation as per ICH guidelines. Hence, it can be routinely used for quantification of THC in bulk drug and formulation.

scholarly journals Development and Validation of a Reversed-Phase HPLC Method for the Estimation of Zolpidem in Bulk Drug and Tablets

2013 ◽  
Vol 2013 ◽  
pp. 1-6
Author(s):  
E. Konoz ◽  
A. H. Mohsen Sarrafi ◽  
R. Abdolahnejad ◽  
M. Bahrami-Zonoz
Keyword(s):  
High Performance ◽  
Dynamic Range ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Hplc Method ◽  
Control Analysis ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Pharmaceutical Dosage Forms ◽  
Bulk Drug

In the present study an isocratic reversed-phase high-performance liquid chromatography method was developed for the estimation of zolpidem in bulk drug and pharmaceutical dosage forms. The quantification was carried out on C18columns. A mixture of acetonitrile-ammonium acetate (pH=8.0, 0.02 M) (60 : 40 v/v) was used as the mobile phase, at flow rate of 1.0 mL/min and the determination wavelength at 245 nm. The retention time of zolpidem was found to be 3–5 min. The validation of the proposed method was carried out for specificity, linearity, accuracy, precision, limit of detection, limit of quantification, and robustness. The linear dynamic range was from 2.5 to 30 μg mL−1. Regression equation was found to bey=0.1416x+0.0183with correlation coefficientr=0.9996. The percentage recovery obtained for zolpidem was greater than 96.5%. Limit of quantification and limit of detection were found to be 2.5 μg mL−1and 0.83 μg mL−1, respectively. The developed method can be used for routine quality control analysis of zolpidem in tablet formulations.

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