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.

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 Determination of Carbamazepine and Its Impurities Iminostilbene and Iminodibenzyl in Solid Dosage Form by Column High-Performance Liquid Chromatography

2010 ◽  
Vol 93 (4) ◽  
pp. 1059-1068 ◽  
Author(s):  
Predrag Lj Džodić ◽  
Ljiljana J ivanovi ◽  
Ana D Proti ◽  
Mira L Zeevi ◽  
Biljana M Joci
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Dosage Form ◽  
Internal Standard ◽  
Hplc Method ◽  
Solid Dosage ◽  
Rp Hplc ◽  
Good Repeatability ◽  
Chemometric Approach

Abstract An accurate and precise RP-HPLC method was developed and validated for the determination of carbamazepine and its impurities iminostilbene and iminodibenzyl in a tablet formulation with fluphenazine as an internal standard. Buffermethanol (50 + 50, v/v) was used as the mobile phase. During validation, specificity, linearity, precision, accuracy, LOD, LOQ, and robustness of the method were tested. The method was proven to be specific against placebo interference. Linearity was evaluated over the concentration range of 100500, 0.050.25, and 0.10.5 g/mL, and the r values were 0.9994, 0.9997, and 0.9979 for carbamazepine, iminostilbene, and iminodibenzyl, respectively. Intraday precision of the method was good, and RSD was below 2 for all analytes. The accuracy of the method ranged from 100.69 to 102.10, 99.76 to 102.66, and 99.26 to 100.08 for carbamazepine, iminostilbene, and iminodibenzyl, respectively. LOD was 0.0125, 0.025, and 0.05 g/mL and LOQ was 0.05, 0.05, and 0.1 g/mL for carbamazepine, iminostilbene, and iminodibenzyl, respectively. Robustness of the method was proven by using a chemometric approach. The method was successfully applied to the analysis of commercially available carbamazepine tablets and showed good repeatability, with RSD below 2.

scholarly journals RP-HPLC Determination of Atomoxetine Hydrochloride in Bulk and Pharmaceutical Formulations

2011 ◽  
Vol 8 (4) ◽  
pp. 1958-1964 ◽  
Author(s):  
H. R. Prajapati ◽  
P. N. Raveshiya ◽  
J. M. Prajapati
Keyword(s):  
Flow Rate ◽  
High Performance ◽  
Pharmaceutical Formulations ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Rp Hplc ◽  
Liquid Chromatographic

A reversed phase high performance liquid chromatographic (RP–HPLC) method was developed and subsequently validated for the determination of atomoxetine hydrochloride in bulk and pharmaceutical formulation. The separation was done by a PerkinElmer Brownlee analytical C8 column (260 mm x 4.6 mm, 5 µm) using methanol: 50 mM KH2PO2buffer (PH adjusted to 6.8 with 0.1 M NaOH), 80:20 v/v as an eluent. UV detection was performed at 270 nm at a flow rate 1.0 mL/min. The validation of the method was performed, and specificity, reproducibility, precision accuracy and ruggedness were confirmed. The correlation coefficient was found to be 0.997 for atomoxetine hydrochloride. The recovery was in the range of 99.94 to 100.98% and limit of quantification was found to be 5.707 µg/mL. The method is simple, rapid, selective and economical too and can be used for the routine analysis of drug in pharmaceutical formulations.

scholarly journals Stability indicating HPLC method for the simultaneous determination of dapagliflozin and saxagliptin in bulk and tablet dosage form

2018 ◽  
Vol 31 (1) ◽  
pp. 39-43 ◽  
Author(s):  
Thiyagarajan Deepan ◽  
Magharla Dasaratha Dhanaraju
Keyword(s):  
Particle Size ◽  
Flow Rate ◽  
Dosage Form ◽  
Correlation Coefficients ◽  
Hplc Method ◽  
Isocratic Elution ◽  
Rp Hplc ◽  
Tablet Dosage ◽  
Detection And Quantification

AbstractA simple, fast, and highly selective RP-HPLC method was developed for the determination of Dapagliflozin (DAP) and Saxagliptin (SAX) in API and tablet dosage form. The separation was done using a Xterra RP18 (4.6×150 mm, 5 μm particle size) column with Acetonitrile: water (60:40). The isocratic elution mode at a flow rate of 1 mL/min, and the analytes were measured at 248 nm. The retention time for DAP and SAX were about 2.091 and 3.249 min, respectively. Calibration curves were found to be linear in the ranges of 100-500 μg/ml for DAP and 50-250 μg/ml for SAX, with correlation coefficients of 0.9998. The detection and quantification values for DAP was 3.0 and 9.98 μg/ml and SAX was 3.02 and 10 μg/ml respectively.

SIMULTANEOUS DETERMINATION OF PARACETAMOL, ACECLOFENAC AND TRAMADOL HYDROCHLORIDE IN PHARMACEUTICAL DOSAGE FORM BY RP-HPLC METHOD

INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (01) ◽  
pp. 35-40
Author(s):  
Rajesh Sharma ◽  
◽  
Mukesh C. Sharma ◽  
Gaurav Vijaywargiya
Keyword(s):  
Flow Rate ◽  
Chromatographic Separation ◽  
Phosphate Buffer ◽  
Mobile Phase ◽  
Dosage Form ◽  
Hplc Method ◽  
Tramadol Hydrochloride ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc

Chromatographic separation of paracetamol, aceclofenac and tramadol hydrochloride was performed on a Chromatopak C-18 column (25 cm x 4.6mm i.d. x 5µm) as stationary phase with a mobile phase composed of phosphate buffer pH 7.0: acetonitrile (65:35 V/V), pH 7.0 (adjusted with triethylamine) at flow rate of 1mL/min. Detection was carried out at 265 nm. The retention times of paracetamol, aceclofenac and Tramadol hydrochloride were found to be 2.7, 4.5 and 6.0 min, respectively. The proposed method was validated for linearity, accuracy, precision, LOD and LOQ. The method was found to be accurate, precise, specific, robust, and linear for the determination of paracetamol, aceclofenac and tramadol hydrochloride in pharmaceutical dosage form.

scholarly journals RP-HPLC Method Development and Validation for Determination of Tigecycline in Bulk and Pharmaceutical Dosage form

2021 ◽  
pp. 273-282
Author(s):  
K. Bhavyasri ◽  
C. H. Mounika ◽  
Narmada Vallakeerthi ◽  
M. Sumakanth
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
Method Development ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Good Precision ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc ◽  
Water Ph

Aims: To develop and validate a new, simple, rapid, precise and accurate Reverse Phase High Performance Liquid Chromatographic (RP-HPLC) method for the quantitative determination of Tigecycline in bulk and pharmaceutical dosage form. Study Design: Place and Duration of the Study: RBVRR women's college of pharmacy, Barkatpura, Hyderabad, between june 2019 and july 2020. Methodology: The RP-HPLC method was developed on Sunsil C18 150 mm x 4.6mm x 5µ column using acetonitrile : water (pH maintained at 3.5 with acetic acid) [70:30] as mobile phase at flow rate 0.8 ml/min and UV detection at 250 nm. Results: Tigecycline exhibited linearity over the concentration range of 5-40 µg/mL (R2 > 0.999). The analytical method showed good precision with % RSD below 2. The method showed suitable accuracy and robustness. Conclusion: Validation of the developed method was done as per International Conference on Harmonization (ICH) Q2R1 guidelines.

scholarly journals QBD APPROACH TO ANALYTICAL METHOD DEVELOPMENT AND ITS VALIDATION FOR ESTIMATION OF LENVATINIB IN BULK AND PHARMACEUTICAL FORMULATION

2021 ◽  
pp. 183-188
Author(s):  
SACHIN A. BABAR ◽  
SUDHAKAR L. PADWAL
Keyword(s):  
Central Composite Design ◽  
Mobile Phase ◽  
High Performance ◽  
Method Development ◽  
Hplc Method ◽  
Factor Screening ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Chromatographic Condition ◽  
Central Composite

Objective: The objective of this research was to develop a simple, very rapid, sensitive, accurate, precise reverse phase High-Performance Liquid Chromatography (RP-HPLC) technique for the estimation of Lenvatinib in bulk and its dosage form. Methods: To perform this study, we employed a central composite design (CCD) to make method robust and effective to create chromatographic database. The factor screening studies were performed using 2-factor 10-runs. The factors were selected as the mobile phase ratio and buffer pH. Results: The desirability value of the optimized model was found to be 0.869 and The optimized chromatographic condition was achieved on Enable C18 analytical column with 0.01M Ammonium acetate buffer pH 3.84: methanol (33.17:66.83 v/v) as the mobile phase and flow rate of 1 ml min-1 and detection wavelength was set to 240 nm. The retention time of Lenvatinib was found to be 5.122 min. Linearity was established for Lenvatinib in the range of 10-50 µg/ml with a correlation coefficient (r2=0.9995). The accuracy values were found to be in the range of 98–102%. Intraday precision and Interday precision were in prescribed (Less than 0.98% RSD). Robustness was found to be less than 1.22% RSD. Conclusion: The proposed method was useful for best analysis of Lenvatinib in Bulk pharmaceutical dosage forms. Central Composite Design was an effective tool for the proposed RP-HPLC method.

scholarly journals RP-HPLC METHOD FOR SIMULTANEOUS ESTIMATION OF RITONAVIR, OMBITASVIR AND PARITAPREVIR IN TABLET DOSAGE FORMS AND THEIR STRESS DEGRADATION STUDIES

2019 ◽  
pp. 193-210
Author(s):  
SYED IBRAHIM BAJE ◽  
B. JYOTHI ◽  
N. MADHAVI
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Array Detector ◽  
Simultaneous Estimation ◽  
Limit Of Quantification ◽  
Rp Hplc

Objective: The objective of the present study was to develop and validate a novel reverse phase high performance liquid chromatographic (RP-HPLC) method, for simultaneous determination of ritonavir (RIT), ombitasvir (OMB) and paritaprevir (PAR) in bulk mixtures, and in tablets. Methods: Determination of the drugs ritonavir (RIT), ombitasvir (OMB), and paritaprevir (PAR), was carried out applying Hypersil BDS C18 column (250 mm X 4.6 mm i.e., 5 µm particle size), with photodiode array detector at λmax of 254 nm. The mobile phase applied for the current study composed of two solvents, i.e. A (0.01N % w/v potassium di-hydrogen orthophosphate buffer, pH 3.0 adjusted with dilute orthophosphoric acid) and B (acetonitrile). The mobile phase was pumped at a flow rate of 1.0 ml/min in the isocratic mode. The validation study with respect to specificity, linearity, precision, accuracy, and robustness, limit of detection (LOD) and limit of quantification (LOQ) was carried out employing the ICH guidelines. Results: Ritonavir, ombitasvir, and paritaprevir showed linearity of response between 12.5-75 μg/ml for ritonavir, 3.125-18.75 µg/ml for ombitasvir and 18.75–112.5 µg/ml for paritaprevir, with a correlation coefficient (R2) 0.999, 0.999,0.999 for RIT, OMB, and PAR respectively. The % recovery obtained was 99.82±0.14 % RIT, OMB 100.03±0.96 % and for 99.96±0.26 % PAR. The LOD and LOQ values for RIT, OMB, PAR were obtained to be 0.02, 0.019and0.02, µg/ml and 0.07, 0.06 and 0.07 µg/ml, respectively. The method also exhibits good robustness for different chromatographic conditions like wavelength, flow rate, mobile phase, and injection volume. Conclusion: The method was successfully employed, for the quantification of RIT, OMB, and PAR, in the quality control of in-house developed tablets, and can be applied for the industrial use.

scholarly journals A Validated RP-HPLC Method for the Estimation of Pizotifen in Pharmaceutical Dosage Form

2012 ◽  
Vol 2012 ◽  
pp. 1-5 ◽  
Author(s):  
M. V. Basaveswara Rao ◽  
A. V. D Nagendrakumar ◽  
Sushanta Maiti ◽  
N. Chandrasekhar
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Dosage Form ◽  
Hplc Method ◽  
Isocratic Elution ◽  
Pharmaceutical Dosage Form ◽  
Reliable Determination ◽  
Rp Hplc ◽  
Ich Guidelines

A simple, selective, linear, precise, and accurate RP-HPLC method was developed and validated for rapid assay of Pizotifen in pharmaceutical dosage form. Isocratic elution at a flow rate of 1.0 mL/min was employed on Chromosil C18 (250 mm × 4.6 mm, 5 μm) column at ambient temperature. The mobile phase consists of methanol : acetonitrile in the ratio of 10 : 90 v/v. The UV detection wavelength was 230 nm, and 20 μL sample was injected. The retention time for Pizotifen was 2.019 min. The percent RSD for accuracy of the method was found to be 0.2603%. The method was validated as per the ICH guidelines. The method can be successfully applied for routine analysis of Pizotifen in the rapid and reliable determination of Pizotifen in pharmaceutical dosage form.

Sign in / Sign up

Export Citation Format

Share Document