Quality by Design (Qbd) Approach to Develop HPLC Method for Estimation of Gliclazide and its Impurity (Gliclazide Impurity A) in Bulk Drug

2019 ◽  
Vol 15 (7) ◽  
pp. 716-723
Author(s):  
Surendran Vijayaraj ◽  
Narahari N. Palei ◽  
Thummala Katyayani
Keyword(s):  
Flow Rate ◽  
Retention Time ◽  
High Performance ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Box Behnken Design ◽  
Injection Volume ◽  
Chromatographic Parameters

Background:Gliclazide Impurity A (GI-A) is one of the gliclazide impurities, as described in the European Pharmacopoeia.Objective:The objective of this study was to develop and validate simple, robust and accurate Reverse- Phase High-Performance Liquid Chromatography (RP-HPLC) method for estimation of gliclazide along with GI-A in bulk by optimising chromatographic parameters using Box Behnken design in response surface methodology.Methods & Results:Box Behnken design was employed for optimizing flow rate, injection volume and strength of the buffer in order to minimize retention time of both gliclazide and GI-A. The optimized strength of orthophosphoric acid buffer in a mixture of Acetonitrile (50:50 v/v), flow rate and injection volume were found to be 25mM, 1mL/min, 20 µL respectively. Linearity was observed in concentration range of 25-150 µg/mL (r2=0.999). The retention time of gliclazide and GI-A was found to be 5.799 minutes and 3.819 minutes, respectively. The limit of detection for Gliclazide and GI-A was found to be 0.0066, and 0.0075 µg/mL and the limit of quantification limit was found to be 0.0202, 0.0228 µg/mL, respectively. The developed method was validated as per the ICH guidelines.Conclusion:The proposed method is useful for best analysis of Gliclazide and GI-A in pharmaceutical dosage forms. QbD approach was found to be an effective tool for optimising chromatographic conditions of the proposed method.

RP-HPLC METHOD FOR ESTIMATION OF LORNOXICAM IN TABLETS AND IN DISSOLUTION SAMPLES USING MASS SPECTROMETRIC COMPATIBLE BUFFERS

INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (07) ◽  
pp. 32-37
Author(s):  
Vijaya Lakshmi Marella ◽  
Chaitanya S. N ◽  
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Mass Spectrometric ◽  
Control Analysis ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Ich Guidelines ◽  
Liquid Chromatographic

A selective and sensitive reverse phase High Performance Liquid Chromatographic method has been developed and validated for the estimation of lornoxicam in bulk, pharmaceutical dosage forms and in dissolution samples. The analysis was performed isocratically on an Inertsil column (250* 4.6 mm, 5 µm) using a mass spectrometric compatible mobile phase of 10 mM ammonium acetate: acetonitrile (50:50 V/V) at a flow rate of 1 mL/min.The detection wavelength was 290 nm. The retention time was found to be 4.573 min for lornoxicam. The linearity of the method has been satisfied with Beer Lambert’s law in the concentration range of 5-25 µg/mL with a correlation coefficient of 0.9988. The mean recoveries assessed for lornoxicam were in the range of 100.39-101.86 %, indicating good accuracy of the method. The limit of detection and limit of quantification were found to be 0.03 and 0.11 µg/mL, respectively. The developed method has been statistically validated in accordance with ICH guidelines and found to be mass spectrometric compatible, simple, precise, and accurate with the prescribed values. Thus, the proposed method was successfully applied for the estimation of lornoxicam in routine quality control analysis of bulk, formulations and in dissolution samples.

DEVELOPMENT OF VALIDATED RP-HPLC METHOD FOR THE QUANTITATIVE ANALYSIS OF CHROMIUM PICOLINATE III IN A DIET VINEGAR FORMULATION

INDIAN DRUGS ◽  
2013 ◽  
Vol 50 (05) ◽  
pp. 48-52
Author(s):  
A Lodhi ◽  
◽  
A Jain ◽  
B. Biswal
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Chromium Picolinate ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

A validated high performance liquid chromatographic method was developed for the determination of chromium picolinate in pharmaceutical dosage forms. The analysis was performed at room temperature using a reversed-phase ODS, 5µm (250×4.6) mm column. The mobile phase consisted of acetonitrile: buffer (60:40 V/V) at a flow rate of 0.5 mL/min. The PDA-detector was set at 264 nm. The developed method showed a good linear relationship in the concentration range from 1.5 – 12.5 µg/mL with a correlation coefficient from 0.999. The limit of detection and limit of quantification were 0.0540513 and 0.1637919 µg/mL respectively.

SIMULTANEOUS DETERMINATION OF FROVATRIPTAN, ALMOTRIPTAN AND ZOLMITRIPTAN IN COMBINED PHARMACEUTICAL DOSAGE FORM BY RP-HPLC METHOD

INDIAN DRUGS ◽  
2012 ◽  
Vol 49 (09) ◽  
pp. 27-32
Author(s):  
V. S Reddy ◽  
◽  
T. E. G. K. Murthy ◽  
N Usha Rani ◽  
R. S Rao ◽  
...  
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

A simple, precise, accurate, reproducible, robust reverse phase high-performance liquid chromatographic method was developed for the simultaneous estimation of frovatriptan, almotriptan and zolmitriptan in bulk and pharmaceutical dosage forms. The method was validated as per ICH and FDA guidelines. Analysis of the drugs was performed on Phenomenex Chromosil C-18 (250 x 4.6 mm, 5 mc) column, in an isocratic mode employing methanol, acetonitrile and THF in the ratio of 46:50:04 (v/v/v) as mobile phase. UV-visible detector at 269 nm was found to be suitable for detection. Linearity was observed in the range of 40-100 ppm.The % recovery was found to be 99.51, 99.69 and 99.34 for frovatriptan, almotriptan and zolmitriptan respectively. The % RSD values for method precision was found to be 0.86, 0.65 and 1.28 for frovatriptan, almotriptan and zolmitriptan respectively. Limit of quantification (LOQ) and limit of detection (LOD) values were found to be 0.15, 0.08 and 0.09 ppm. and 0.05, 0.02, 0.03 for frovatriptan, almotriptan and zolmitriptan respectively.

scholarly journals Research Article on Development and Validation of RP-HPLC Method for Estimation of Canagliflozin

2019 ◽  
Vol 11 (02) ◽  
pp. 85-92
Author(s):  
Gudipally. Mounika ◽  
K. Bhavya Sri ◽  
R. Swethasri ◽  
M. Sumakanth
Keyword(s):  
Retention Time ◽  
High Performance ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Pharmaceutical Dosage Form ◽  
Validation Parameters ◽  
Liquid Chromatography Method ◽  
Development And Validation

To develop an accurate, precise, specific high performance liquid chromatography method for quantification of Canagliflozin in bulk and dosage forms. A C18 column (250mm X 4.6mm; 5μm phenomenex) was used with mobile phase containing Acetonitrile-0.1% sodium acetate buffer (pH-4.6), (20:80) in isocratic mode. The flow rate maintained was 1.0ml/min and the U.V detector was operated at 291nm. The retention time of Canagliflozin was 3.307min and showed a good linearity in concentration range of 2-14μg/ml with correlation coefficient of 0.999. The average percent recovery was found to be 99.98%. The developed method follows validation parameters such as system suitability, linearity, precision, accuracy, limit of detection and limit of quantification and robustness as per ICH guidelinesQ2(R1). The proposed method was found to provide faster retention time with sharp resolution with linearity at a lowest concentration as compared to previous methods and this method is validated as per International conference on harmonization guidelines and successfully applied for bulk and pharmaceutical dosage form.

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.

RP-HPLC Assay for Estimation of Pitavastatin in Bulk and Pharmaceutical Dosage Forms

2014 ◽  
Vol 7 (1) ◽  
pp. 2346-2349
Author(s):  
K Tirumala ◽  
CH.V.S Gautam ◽  
J Gangadhar ◽  
M Jayajeevitha ◽  
Vanitha Prakash K
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Dosage Forms ◽  
Hplc Method ◽  
Detector Response ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Bulk Drug

Reverse phase high performance liquid chromatographic (RP-HPLC) method was developed and validated for the estimation of pitavastatin in tablet dosage form. A Phenomenex Luna C18, 150×4.6 mm i.d, 5 µm particle size with mobile phase consisting of buffer 0.01M potassium dihydrogen ortho phosphate pH (3.75) adjusted with dilute orthophosphoric and acetonitrile in the ratio of 20:80 v/v was used. The flow rate was 1.2 mL/min and eluents were monitored at 248 nm. The retention time was 4.1min. The detector response was linear in the concentration of 25-150 µg/mL, with the regression coefficient of 0.9998. Quantification was done by calculating area of the peak and the limit of detection and limit of quantification were 1.9 µg/mL and 5.7 µg/mL respectively. The percentage assay of pitavastatin was 101.1%. The results of study showed that the proposed RP-HPLC method is simple, rapid, precise and accurate which is useful for the routine determination of pitavastatin in bulk drug and in its pharmaceutical dosage forms.

DEVELOPMENT AND VALIDATION OF RP-HPLC-PDA METHOD FOR THE ESTIMATION OF FENSPIRIDE HYDROCHLORIDE IN BULK AND PHARMACEUTICAL DOSAGE FORMS.

INDIAN DRUGS ◽  
2015 ◽  
Vol 52 (01) ◽  
pp. 20-25
Author(s):  
S. M Samyuktha ◽  
◽  
P. G Prasanthi ◽  
K Mahesh ◽  
B. N Nalluri ◽  
...  
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Dosage Forms ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Development And Validation ◽  
Tablet Dosage ◽  
Liquid Chromatographic

A simple, selective, accurate High Performance Liquid Chromatographic (HPLC) method was developed and validated for the analysis of Fenspiride hydrochloride in bulk and tablet dosage forms. Chromatographic separation was achieved isocratically using a C18 reverse phase column [Inertsil C18 column (250×4.6mm, 5μm)] utilizing a mobile phase containing 10mM Ammonium acetate: Acetonitrile (50:50 v/v) at a flow rate of 1 mL/min. The eluents were monitored at wavelength of 210 nm for a run time of 7 minutes at ambient temperature. The average retention time of the drug was found to be 4.6 minutes. The developed method was validated as per ICH guidelines to ascertain the reproducibility of the method. The method was found to be linear in the concentration range of 10-50 μg/mL with a good correlation coefficient of 0.998. The limit of detection (LOD) and limit of quantification (LOQ) were 0.007 and 0.021 μg/mL and the percentage recovery and assay were found to be 99.315 and 98.97%. Specificity with placebo by 3 D plots showed that the method was specific and free from interfering substances. Therefore, the fully validated method was good enough to carry out routine analysis of Fenspiride in bulk and tablet formulations.

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.

Chemometric Approach to Develop and Validate RP-HPLC Method for Estimation of Erlotinib Hydrochloride in Nano Structured Lipid Carriers

2020 ◽  
Vol 16 (2) ◽  
pp. 210-219
Author(s):  
Narahari Narayan Palei ◽  
Surendran Vijayaraj ◽  
Kuppam Lathasri ◽  
Devalapalli Archana ◽  
Ponnusamy Rajavel
Keyword(s):  
Flow Rate ◽  
Retention Time ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Nanostructured Lipid Carriers ◽  
Asymmetry Factor ◽  
Forced Degradation ◽  
Injection Volume ◽  
Rp Hplc ◽  
Chemometric Approach

Background: Erlotinib hydrochloride is a novel drug for the treatment of lung cancer. Objective: The objective of the present study was to design an uncomplicated and precise reverse phase high-performance liquid chromatography (RP-HPLC) method and optimize the chromatographic parameters using response surface methodology derived from Box Behnken design. The optimized method was validated for estimating Erlotinib from bulk and nanostructured lipid carriers (NLCs) formulation. Methods: Independent variables such as flow rate, injection volume and strength of the buffer were optimized in order to decrease retention time and curtail asymmetry factor of Erlotinib. Forced degradation studies were done to determine the stability of the drug. The developed method was validated as per ICH guidelines. Results: The optimized strength of ortho-phosphoric acid buffer by blending with Acetonitrile (80:20 v/v), flow rate and injection volume were found to be 25mM, 1ml/min, 20µL respectively. Linearity was observed in the concentration range of 1-6 µg/mL. The retention time of Erlotinib was found to be 3.717 minutes. The limit of detection and limit of quantification for Erlotinib were found to be 0.01ng/ml and 1ng/ml, respectively. Conclusion: The proposed method was found to be a simple and the best method for analysing Erlotinib in nanostructured lipid carriers. Chemometric approach was employed as an effective tool for optimising the chromatographic conditions of the proposed 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.

Sign in / Sign up

Export Citation Format

Share Document