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.

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.

scholarly journals Box-Behnken Assisted Validation and Optimization of an RP-HPLC Method for Simultaneous Determination of Domperidone and Lansoprazole

Separations ◽  
2021 ◽  
Vol 8 (1) ◽  
pp. 5
Author(s):  
Mohd Afzal ◽  
Mohd. Muddassir ◽  
Abdullah Alarifi ◽  
Mohammed Tahir Ansari
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Box Behnken Design ◽  
Rp Hplc ◽  
System Suitability ◽  
Method Optimization ◽  
Key Variables

A highly specific, accurate, and simple RP-HPLC technique was developed for the real-time quantification of domperidone (DOMP) and lansoprazole (LANS) in commercial formulations. Chromatographic studies were performed using a Luna C8(2), 5 μm, 100Å, column (250 × 4.6 mm, Phenomenex) with a mobile phase composed of acetonitrile/2 mM ammonium acetate (51:49 v/v), pH 6.7. The flow rate was 1 mL·min−1 with UV detection at 289 nm. Linearity was observed within the range of 4–36 µg·mL−1 for domperidone and 2–18 µg·mL−1 for lansoprazole. Method optimization was achieved using Box-Behnken design software, in which three key variables were examined, namely, the flow rate (A), the composition of the mobile phase (B), and the pH (C). The retention time (Y1 and Y3) and the peak area (Y2 and Y4) were taken as the response parameters. We observed that slight alterations in the mobile phase and the flow rate influenced the outcome, whereas the pH exerted no effect. Method validation featured various ICH parameters including linearity, limit of detection (LOD), accuracy, precision, ruggedness, robustness, stability, and system suitability. This method is potentially useful for the analysis of commercial formulations and laboratory preparations.

scholarly journals Validated Stability Indicating RP-HPLC Method for Simultaneous Estimation of Codeine Phosphate and Chlorpheniramine Maleate from Their Combined Liquid Dosage Form

2013 ◽  
Vol 2013 ◽  
pp. 1-7 ◽  
Author(s):  
Ramakrishna Kommana ◽  
Praveen Basappa
Keyword(s):  
Limit Of Detection ◽  
Degradation Products ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Forced Degradation ◽  
Codeine Phosphate ◽  
Chlorpheniramine Maleate ◽  
Combination Drug ◽  
Stability Indicating ◽  
Rp Hplc

The present paper describes the development of quick stability indicating RP-HPLC method for the simultaneous estimation of codeine phosphate and chlorpheniramine maleate in the presence of its degradation products, generated from forced degradation studies. The developed method separates codeine phosphate and chlorpheniramine maleate in impurities/degradation products. Codeine phosphate and chlorpheniramine maleate and their combination drug product were exposed to acid, base, oxidation, dry heat, and photolytic stress conditions, and the stressed samples were analysed by proposed method. The proposed HPLC method utilizes the Shimadzu HPLC system on a Phenomenex C18 column (, 5 μ) using a mixture of 1% o-phosphoric acid in water : acetonitrile : methanol (78 : 10 : 12) mobile phase with pH adjusted to 3.0 in an isocratic elution mode at a flow rate of 1 mL/min, at 23°C with a load of 20 μL. The detection was carried out at 254 nm. The retention time of codeine phosphate and chlorpheniramine maleate was found to be around 3.47 min and 9.45 min, respectively. The method has been validated with respect to linearity, robustness, precision, accuracy, limit of detection (LOD), and limit of quantification (LOQ). The developed validated stability indicating HPLC method was found to be simple, accurate, and reproducible for the determination of instability of these drugs in bulk and commercial products.

scholarly journals RP-HPLC Determination of Raloxifene in Pharmaceuticl Tablets

2006 ◽  
Vol 3 (1) ◽  
pp. 60-64 ◽  
Author(s):  
P. Venkata Reddy ◽  
B. Sudha Rani ◽  
G. Srinu Babu ◽  
J. V. L. N. Seshagiri Rao
Keyword(s):  
Flow Rate ◽  
Retention Time ◽  
Mobile Phase ◽  
Dosage Forms ◽  
Hplc Method ◽  
Reverse Phase Hplc ◽  
Reverse Phase ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc

A reverse phase HPLC method is developed for the determination of Raloxifene in pharmaceutical dosage forms. Chromatography was carried out on an inertsil C18 column using a mixture of acetonitrile and phosphate buffer (30:70 v/v) as the mobile phase at a flow rate of 1 mL/min. Detection was carried out at 290 nm .The retention time of the drug was 10.609 min. The method produced linear responses in the concentration range of 0.5-200 µg/mL of Raloxifene. The method was found to be applicable for determination of the drug in tablets.

scholarly journals METHOD DEVELOPMENT AND VALIDATION FOR THE ESTIMATION OF ENTECAVIR IN BULK AND PHARMACEUTICAL DOSAGE FORMS BY RP-HPLC

2017 ◽  
pp. 107-111
Author(s):  
Swathi P. ◽  
S. Vidyadhara ◽  
R. L. C. Sasidhar ◽  
K. Kalyan Chakravarthi
Keyword(s):  
Flow Rate ◽  
Dosage Forms ◽  
Hplc Method ◽  
Forced Degradation ◽  
Uv Detector ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Validation Parameters ◽  
Degradation Studies

Objective: The objective and purpose of the analysis have sensibly assessed by selecting of a rapid and sensitive RP-HPLC method for Entecavir in bulk and pharmaceutical dosage form by using the most commonly employed C-18column with UV detection.Methods: In estimation by RP-HPLC method Agilent 1120 compact LC system with variable programmable UV detector and Rheodyne injector with 20 µl fixed loop was used for the chromatographic separation. The mode of operation was isocratic with the components of a solution consisting of methanol: acetonitrile(70:30v/v) and triethanolamine (2-4drops)at the flow rate of 1.2 ml/min and run time was 10 min. Forced degradation studies were conducted to evaluate the stability and specificity of the method along with the validation parameters.Results: Validation parameters of HPLC were found at a detection wavelength of 255 nm. Linearity was observed with the concentration range (Beer’s law range) 20-100µg/ml with R2=0.9991. Robustness with detection wavelengths 253 and 257 nm with a flow rate of 1 ml/min and 1.4 ml/min showed good results. The retention time of the drug was 2.64 min and assay showed 98.1%.Conclusion: The proposed RP-HPLC method was validated as per the ICH Q2B Guidelines, and was found to be applicable for routine quantitative analysis of Entecavir by RP-HPLC using UV detector in pharmaceutical dosage forms. The results of linearity, precision, accuracy and specificity, were proved, that does not exceed certain specified limits. The method provides selective quantification with no interference from other formulation excipients. The proposed method was highly sensitive, reproducible, reliable, robust and specific. Therefore, this method is a simple, rapid analysis may actually be more desirable than a more complicated and time-consuming process. The degradation studies at various stress conditions like thermal and hydrolytic, drug gets degraded at a temperature of 80 °c and refluxing with water at 70 °c for 24hours. 

scholarly journals Fasten, simple, and specific stability of the avant-garde RP-HPLC method for estimation and validation of nystatin in pharmaceutical formulations

2019 ◽  
Vol 10 (4) ◽  
pp. 3717-3727
Author(s):  
Dawood CH. Al-Bahadily ◽  
Rasool Chaloob ◽  
Kulood H. Oudah ◽  
H. N. K. AL-Salman ◽  
Falah Hassan Shari ◽  
...  
Keyword(s):  
Flow Rate ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Avant Garde ◽  
Rp Hplc ◽  
Specificity And Sensitivity ◽  
Stress Degradation ◽  
The Stability

In this study, a simple and reliable stability-indicating RP-HPLC method was developed and validated for the analysis of Nystatin in the pharmaceuticals. The chromatographic separation was performed in the isocratic mode on an Ion Pac column; Arcus EP‑C18; 5μm, 4.6×250 mm, 30 °C) using a mobile phase consisting of ammonium acetate 0.05 M buffer/ Methanol mixture (30:70) and a flow-rate of 1.0 mL/min with UV detection at 305 nm. The flow rate was set at 1.0 mL/min. The HPLC analysis method was validated in terms of linearity, precision, accuracy, specificity, and sensitivity, according to International Conference on Harmonization (ICH) guidelines. The results indicated that the retention time was 8 min, and no interferences were observed from the formulation excipients and stress degradation products.  The specificity, linearity, precision, accuracy, LOD, and LOQ of the method were validated. The method was linear over the range of 5–500 μg/mL with an acceptable correlation coefficient (R2 = 0.9996). The method’s limit of detection (LOD) and quantification (LOQ) were 0.01 and 0.025 μg/mL, respectively. The results indicate that this validated method can be used as an alternative method for the assay of nystatin. This validated HPLC method could be used for routine analysis, quality control, and the stability of analysis of Nystatin formulations.

scholarly journals Development and Validation of RP-HPLC for Estimation of Neratinib in Bulk and Tablet Dosage Form

2019 ◽  
Vol 11 (02) ◽  
Author(s):  
M Lakshmi Kanth ◽  
B Raj Kama
Keyword(s):  
Flow Rate ◽  
Retention Time ◽  
Chromatographic Separation ◽  
Mobile Phase ◽  
Dosage Form ◽  
Hplc Method ◽  
Rp Hplc ◽  
Monopotassium Phosphate ◽  
Development And Validation ◽  
Tablet Dosage

An accurate RP-HPLC method developed for the estimation of Neratinib in bulk and tablet dosage form. The method is and validated for parameters linearity, accuracy, suitability, specificity, precession, LOD, LOQ and robustness. An Altima column (150 mm × 4.6 mm × 5μ) used for chromatographic separation within a runtime of 6 min. The mobile phase buffer (monopotassium phosphate) and acetonitrile (60:40 v/v) with 0.1% formic acid is used. The flow rate maintained at 1.0 ml/min with the effluents monitored at 215 nm. The Neratinib analyzed at retention time of 4.001. The concentration linear over 30-180μg/ml with regression equation y = 6065.6x + 795.43 and regression co-efficient 0.999.

scholarly journals A VALIDATED STABILITY INDICATING RP-HPLC METHOD FOR ESTIMATION OF TOLFENAMIC ACID IN PRESENCE OF ITS PHARMACOPOEIAL IMPURITIES

2019 ◽  
pp. 264-270
Author(s):  
ADISON FERNANDES ◽  
SANJAY PAI P. N.
Keyword(s):  
Oxidative Stress ◽  
Correlation Coefficient ◽  
Flow Rate ◽  
Hplc Method ◽  
Tolfenamic Acid ◽  
Stress Conditions ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Related Impurities ◽  
Rp Hplc

Objective: The proposed research work was conducted to develop a single reverse-phase high-performance chromatography (RP-HPLC) method capable of separating two Pharmacopoeial related impurities as well as degradation product of Tolfenamic acid (TA). The drug was subjected to various stress conditions recommended under ICH Q1A (R2) guidelines. Methods: The desired separation of two Pharmacopoeial impurities and one degradant generated under oxidative stress was carried out using Sunfire ODS C-18 (250 x 4.6 mm, 5 µm) column maintained at 40 °C. Isocratic elution was carried out using acetonitrile and ammonium dihydrogen orthophosphate buffer (10 mmol, pH 2.5) in the ratio of 80:20 v/v. The detection was carried out at 205 nm using flow rate of 1 ml/min. The developed method was validated as per ICH Q2 (R1) guidelines for specificity, linearity, accuracy, precision, Limit of detection (LOD), Limit of Quantification (LOQ) and robustness. Results: Linearity response of TA was found at a concentration range of 10-100µg/ml, with a correlation coefficient of 0.9987. The Pharmacopoeial impurity A and impurity B showed linearity results at concentration of 0.1-1µg/ml, with correlation coefficient of 0.9984 for Impurity A and 0.9989 for Impurity B. The % recovery during accuracy studies for TA and the two impurities were within the acceptance range of 95-105%. LOD and LOQ for TA were found to be 4.561µg/ml and 133.771µg/ml respectively. For impurity A, LOD and LOQ were found to be 0.035 µg/ml and 0.106 µg/ml and for Impurity B, LOD and LOQ were 0.042 µg/ml and 0.128 µg/ml. With slight variation of organic phase in mobile phase and flow rate the method exhibited good robustness. Under forced degradation studies the drug was found stable under hydrolytic, photolytic and thermal stress conditions, but was found susceptible for degradation under oxidative stress with appearance of a degradant peak. From on the RRT values of Pharmacopoeial impurities and the formed degradant it was inferred that the developed method is selective for the drug in the presence of impurities or degradants. Conclusion: The developed stability-indicating method is found to be simple, rapid, accurate, precise and robust as compared to other proposed methods while determining TA in presence of its Pharmacopoeial impurities and degradation products. Hence the developed method can be used for analysis of stability samples of TA in presence of its related impurities.

A new simple RP-HPLC Method development, Validation and Forced degradation studies of Bilastine

2021 ◽  
pp. 183-187
Author(s):  
Khushbu K. Patel ◽  
Arati M. Patel ◽  
C. N. Patel
Keyword(s):  
Retention Time ◽  
Dosage Form ◽  
Method Development ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Forced Degradation ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Ich Guidelines ◽  
Hplc Method Development

A new simple, rapid, accurate and precise method for estimation of Bilastine in pharmaceutical dosage form by reverse phase liquid chromatography. The developed method employed mobile phase was Acetonitrile and Ammonium acetate pH 5.0 adjusted with glacial acetic acid with 85:15% v/v and flow rate 1.0ml/min. Method was developed using column C18 Water (150 × 4.6mm, 5µm) and detection wavelength was 215nm. The retention time was found to be 2.519 min. the proposed method was successfully applied to the determination of Bilastine in dosage form. High linearity of developed method was confirmed over concentration range of 25- 150 µg/ml and co-relation co-efficient is 0.996. The percentage RSD for precision and accuracy of the method was found to be less than 2%. The recovery was in the range of 99 – 102% and limit of detection was found to be 0.45µg/ml and limit of quantification was found to be 1.20µg/ml. Bilastine was found to degrade under acid and oxidation conditions. There was no interference of excipient and degradation product in retention time so method was specific. Analytical parameter such as precision, accuracy, limit of detection, limit of quantification and robustness were determined according to international Conference on Harmonization (ICH) guidelines.

scholarly journals Stability-Indicating Validated Novel RP-HPLC Method for Simultaneous Estimation of Methylparaben, Ketoconazole, and Mometasone Furoate in Topical Pharmaceutical Dosage Formulation

2013 ◽  
Vol 2013 ◽  
pp. 1-9 ◽  
Author(s):  
Chinmoy Roy ◽  
Jitamanyu Chakrabarty
Keyword(s):  
Limit Of Detection ◽  
Hplc Method ◽  
Mometasone Furoate ◽  
Simultaneous Estimation ◽  
Forced Degradation ◽  
Solution Stability ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Dosage Formulation

A simple, specific, precise, and accurate RP-HPLC method has been developed and validated for simultaneous estimation of Methylparaben (MP), Ketoconazole (KT), and Mometasone Furoate (MF) topical pharmaceutical dosage formulation. The separation was achieved by Waters X Terra C18 column using mobile phase consisting of buffer (triethyl amine in water, pH adjusted to 6.5 with glacial acetic acid)-acetonitrile (40 : 60, v/v) at a flow rate of 1.5 mL/min and detection at 250 nm. The method showed linearity with correlation coefficient <0.9999 over the range of 0.12–15.2 μg/mL, 0.67–149.4 μg/mL, and 0.42–7.6 μg/mL for MP, KT, and MF, respectively. The mean recoveries were found to be in the range of 99.9–101.1% for all the components. The method was validated as per the ICH guidelines for linearity, limit of detection, limit of quantification, accuracy, precision, robustness and solution stability. Stability indicating capability of the developed method was established by analyzing forced degradation of samples in which spectral purity of MP, KT, and MF along with separation of degradation products from analytes peak was achieved. The method can be successfully applied for routine analysis of quantitative determination of MP, KT, and MF in pharmaceutical dosage form.

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