scholarly journals ANALYTICAL QUALITY-BY-DESIGN (AQBD) APPROACH FOR THE DEVELOPMENT AND VALIDATION OF RP-HPLC METHOD FOR THE ESTIMATION OF LAMOTRIGINE IN BULK AND TABLET FORMULATION

2021 ◽  
Vol 10 (5) ◽  
pp. 3591-3596
Author(s):  
Manisha P. Puranik
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
High Performance ◽  
Quality By Design ◽  
Active Pharmaceutical Ingredient ◽  
Reversed Phase ◽  
Hplc Method ◽  
Analytical Technique ◽  
Rp Hplc ◽  
Ich Guideline

The current analytical exploration illustrated developing a reversed-phase high-performance liquid chromatography (RP-HPLC) technique and consequent substantiation for analyzing lamotrigine (LAM) active pharmaceutical ingredient (API) using a Quality-by-design (QbD) approach (Central Composite Design), in bulk product as well as in the tablet formulations. In this experiment, based on systematic scouting, four key components (viz., mobile phase, column, flow-rate, and wavelength) were studied by the RP-HPLC method. 13 experimental runs were done with acetonitrile (ACN) (40-60% v/v) having flow-rate in the range 0.8 mL/min to 1.2 mL/min. The proposed analytical method was thoroughly corroborated in terms of ruggedness linearity, robustness, accuracy, and precision in accordance with ICH guideline Q2A and ICH guideline Q2B. Under the optimum chromatographic environment; Intersil C8 column of 250 mm length, 4.6 mm (i.d.); 20 μL injection volume; and mobile phase ACN: Methanol (60:40 v/v), a retention time of 2.542 min was noticed at 220 nm detection wavelength. The method was found to be extremely reproducible, accurate, linear, precise, robust, and economically adequate to execute the estimation. The intended analytical technique was thoroughly assessed through statistical tools and could be an imperative concern for the habitual scrutiny of LAM in bulk products and its formulation.

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

SIMULTANEOUS ESTIMATION OF CURCUMIN AND GEFITINIB IN BULK AND TISSUE SAMPLES (PLASMA AND BRAIN HOMOGENATE) BY RP-HPLC: APPLICATION TO A DISTRIBUTION STUDY

INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (07) ◽  
pp. 59-68
Author(s):  
H Mahajan ◽  
S Savale ◽  
P Nerkar ◽  
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Internal Standard ◽  
Brain Homogenate ◽  
Reversed Phase ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Bulk Analysis ◽  
Experimental Conditions ◽  
Rp Hplc

The present study was aimed at developing a Reversed-Phase High-Performance Liquid Chromatography (RP-HPLC) method for simultaneous determination of curcumin (CRM) and gefitinib (GFT) in bulk, plasma and brain homogenate. hydrochlorothiazide was used as an internal standard (IS). A new simple, rapid, selective, precise and accurate RP-HPLC method has been developed. The separation was achieved by using C-18 column (Qualisil BDS C18, 250 mm x 4.6 mm I.D.) coupled with a guard column of silica, mobile phase consisted of acetonitrile: water with 0.1% formic acid (30:70 v/v). The flow rate was 0.2 ml/min and the drug was detected using PDA detector at the wavelength of 242 nm. The experimental conditions, including the diluting solvent, mobile phase composition, column saturation and flow rate, were optimised to provide high-resolution and reproducible peaks. The method was developed and tested for linearity range of 10-60 μg/mL for bulk analysis and 200-800 ng/mL for plasma and brain homogenate. The developed method was validated as per ICH guidelines, in terms of linearity, application of the proposed method to bulk sample, recovery, precision, repeatability, ruggedness, sensitivity (LOD and LOQ) and robustness and stability study (short and long-term stabilities, freeze/thaw stability, post-preparative). The low value of % RSD showed that the method was precise within the acceptance limit of 2%. The developed method was successfully applied for the analysis of the drug in bulk as well as various marketed formulation and drug in plasma and brain distribution studies.

Degradation Profiling of Lisinopril and Hydrochlorothiazide by RP- HPLC method with QbD Approach

2021 ◽  
pp. 270-274
Author(s):  
Kalleshvar P. Jatte ◽  
R. D. Chakole ◽  
M. S. Charde
Keyword(s):  
Particle Size ◽  
Quality Control ◽  
Flow Rate ◽  
Mobile Phase ◽  
Dosage Form ◽  
Quality By Design ◽  
Hplc Method ◽  
Rp Hplc ◽  
Tablet Dosage ◽  
Gradient Mode

RP-HPLC method was developed for the estimation of Lisinopril and Hydrochlorothiazide in tablet dosage form with the help of Quality by Design (QbD) approaches. In this method concentration of each drug was obtained by using the absorptivity values calculated for drug wavelength 226.0 nm and solving the equation. The RP-HPLC method was performed C18-(100mm x 4.6 mm,)2.5 μm particle size in gradient mode, and the sample was analysed using methanol 45.0 ml and 55.0 ml (pH 3.3 0.05% OPA with TEA) as a mobile phase at a flow rate of 0.8 ml/min and detection at nm. By the retention time for Lisinopril and Hydrochlorothiazide found 3.39 and 4.59 min respectively. Validation related the method is specific, rapid, accurate, precise, reliable, and reproducible. Calibration plots by both HPLC were linear over the 5-25 and 12.5-62.5 μg/ml for Lisinopril and Hydrochlorothiazide respectively, and recoveries from tablet dosage form were between 99.02 and 100.00 %. The method can be used for routine of the quality control in pharmaceuticals. The degradation profiling of Lisinopril and Hydrochlorothiazide were also carried out.

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 Reverse-phase High-Performance Liquid Chromatography Method Development and Validation for Estimation of Glimepiride in Bulk and Tablet Dosage Form

2020 ◽  
Vol 11 (02) ◽  
pp. 296-302
Author(s):  
Aseem Kumar ◽  
Anil Kumar Sharma ◽  
Rohit Dutt
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Flow Rate ◽  
Retention Time ◽  
Mobile Phase ◽  
High Performance ◽  
Hplc Method ◽  
Reverse Phase ◽  
Rp Hplc ◽  
Development And Validation

The present work demonstrates a simple, rapid, precise, specific, and sensitive reverse-phase high-performance liquid chromatography (RP-HPLC) method for analyzing glimepiride in pure and tablet forms. The present method was developed using a C18 column 150 × 4.6 mm, with 5 μm, and packing L1 maintained at a temperature of 30°C. The mobile phase was prepared by dissolving 0.5 gram of monobasic sodium phosphate in 500 mL of distilled water, pH of the solution adjusted to 2.1 to 2.7 with 10% phosphoric acid, and added 500 mL of acetonitrile. The mobile phase was pumped in the highperformance liquid chromatography (HPLC) system at a flow rate of 1 mL/min, and separation was carried out at 228 nm, using an ultraviolet (UV) detector. The chromatographic separation was achieved with peak retention time (RT) at about 9.30 minutes, and the method was found to be linear over a concentration range of 40 to 140 μg/mL. The specificity of the method represented no interference of the excipients during the analysis, and stability testing after 24 hours also showed that the method is suitable and specific. The accuracy was between 99.93 to 99.96%, with limit of detection (LOD) and limit of quantitation (LOQ) being 0.354 μg/mL, 1.18 μg/mL, respectively. Satisfactory results were found for precision and robustness parameters during the development and validation stage for the analytical method. The proposed method was also adopted for the analysis of glimepiride tablets to improve the overall quality control. Using this method, symmetric peak shape was obtained with reasonable retention time. The retention time of glimepiride for six repetitions is 9.3 ± 0.1 minutes; the run time is 21 minutes. The proposed RP-HPLC method is a modification of the United States Pharmacopeia (USP) method, and it was found to be valid for glimepiride within concentration ranges 40 to 140 μg/mL, using C18 analytical columns, and isocratic elution with UV detection, and at 1 mL/min of flow rate.

scholarly journals DEVELOPMENT AND VALIDATION OF REVERSED-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR GABAPENTIN AND ITS RELATED SUBSTANCES IN CAPSULE DOSAGE FORM AND EXCIPIENT COMPATIBILITY STUDIES

2018 ◽  
Vol 11 ◽  
Author(s):  
Afroz Patan
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Dosage Form ◽  
Reversed Phase ◽  
Hplc Method ◽  
Compatibility Studies ◽  
Compound A ◽  
Related Substances ◽  
Rp Hplc ◽  
Excipient Compatibility

Objective: A simple, accurate, precise, and reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed and validated for gabapentin (GBP) and its related substances in the capsule dosage form and excipient compatibility studies. Methods: The review of literature indicates that various methods have been reported for the estimation of GBP. When some excipients were used for GBP, it produced degradation product called lactam due to the presence of more water content. Hence, a novel RP-HPLC method has been developed for studying excipient compatibility and related substances of GBP in capsule dosage form using excipients such as lactose anhydrous and dried maize starch which is having less water activity. Waters Alliance e2695 separation module with ultraviolet/photodiode array (UV/PDA) detector with Inertsil C8 (250 mm×4.6 mm); 5 μm with an injection volume of 50 μl is injected and eluted with the (gradient program) mobile Phase A buffer: acetonitrile (940:60) and mobile phase B buffer: acetonitrile (700:300) pH 6.9 with 5 N potassium hydroxide which is pumped at a speed of 1.5 ml/min and detected by UV/PDA detector at 210 nm. The peaks of GBP and GBP-related compound A are well separated at 6.7 min and 34.5 min, respectively. Results: The method developed was approved for various parameters such as accuracy, specificity, precision, intermediate precision, range, linearity, robustness, limit of detection, limit of quantification, steadiness, and system suitability according to the International Conference on Harmonization guidelines. The results got were according to the acceptance criteria. Conclusion: The technique proposed was assured for detection of related substances in the marketed formulation and could be used for the routine analysis of GBP and GBP-related compound A in the capsule dosage form.

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 Development and Validation of rp-HPLC Method of Cabozantinib in Active Pharmaceutical Ingredient and Pharmaceutical Dosage form

2021 ◽  
pp. 81-90
Author(s):  
Amruta A. Chaudhary ◽  
Ashwini V. Shelke ◽  
Anil G. Jadhav
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Dosage Form ◽  
Limit Of Detection ◽  
Active Pharmaceutical Ingredient ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc

A specific, accurate rp-HPLC (reversed-phase high performance liquid chromatographic) method was developed for the quantification of Cabozantinib. The effective separation was achieved through reversed-phased C18 column 4.6 x 250 mm, 5µm using a mobile phase Methanol: phosphate buffer (ph. 3.00) with orthophosphoric acid (OPA) (55:45 % v/v). The flow rate of the mobile phase was found to be 0.8 mL/min. The detection was carried at a wavelength of 244 nm. The retention time of Cabozantinib was found to be 3.702 min. The correlation coefficient was found to be 0.9999. The developed method was accurately validated in the terms of accuracy, linearity range, precision, system suitability, robustness, limit of detection and limit of quantification. The details presented in this test will be useful for industrial application for determining Cabozantinib in active pharmaceutical ingredient and pharmaceutical dosage form.

scholarly journals A new RP-HPLC method as an auxiliary tool for optimization of sample preparation procedures for tracing of PPCPs of different hydrophilicities

2021 ◽  
Vol 71 (2) ◽  
pp. 305-315
Author(s):  
Omar J. Portillo-Castillo ◽  
Rocío Castro-Ríos ◽  
Abelardo Chávez-Montes ◽  
Azucena González-Horta ◽  
Norma Cavazos-Rocha ◽  
...  
Keyword(s):  
Sample Preparation ◽  
High Performance ◽  
Reversed Phase ◽  
Hplc Method ◽  
Suitable Alternative ◽  
Analytical Technique ◽  
Rp Hplc ◽  
Mobile Phases ◽  
Wide Range ◽  
Gradient Mode

AbstractRecently, pharmaceutical and personal care products (PPCPs) have received considerable attention because of their increasing use. Analysis of PPCPs presents a significant analytical challenge, with high-performance liquid chromatography (HPLC) in reversed-phase mode, as the most widely used analytical technique. To facilitate the optimization of the procedures that are applied in the early stages of sample preparation, a simple and fast HPLC method is proposed in this work for the separation of some PPCPs with a wide range of hydrophilicity. Two columns were evaluated (Atlantis dC18 and Discovery HS F5); as for mobile phases: a formate buffer (40 mmol L−1, pH 4) and methanol were tested in a gradient mode. The fluorinated column allowed better separation in a shorter time and better resolution for all analytes (Rs > 1). The proposed method delivered good performance for the tracing of PPCPs and is a suitable alternative to traditional C18-based HPLC methods.

scholarly journals EFFECTS OF PH AND AMOUNT OF ACETONITRILE ON THE SEPARATION OF CANNABINOIDS

2021 ◽  
pp. 70-76
Author(s):  
EVA TEJADA ◽  
JANIS VELLA SZIJJ ◽  
MIRIANA CACHIA ◽  
PAULINE FALZON ◽  
LILIAN M AZZOPARDI ◽  
...  
Keyword(s):  
Stationary Phase ◽  
Flow Rate ◽  
Retention Time ◽  
Mobile Phase ◽  
High Performance ◽  
Reversed Phase ◽  
Hplc Method ◽  
High Throughput Analysis ◽  
Chromatographic Peaks ◽  
Chromatographic Parameters

Objective: During reversed-phase high-performance liquid chromatography (HPLC) analyses, optimization of separation can be achieved by selecting appropriate chromatographic conditions. The retention time, peak shape, and peak size of chromatographic peaks are dependent on amount of organic modifier in the mobile phase and buffer pH. The aim of this study was to investigate the effects of varying pH, acetonitrile composition and flow rate of the mobile phase, and temperature of the stationary phase and wavelength in the development of a method to separate Δ9 tetrahydrocannabinol, cannabidiol, and cannabinol. Methods: Mobile phases with different buffer pHs and acetonitrile composition were used with ultraviolet (UV) detection wavelength of 220 nm and 228 nm. The AUPs and retention times were observed using different mobile phase flow rates and stationary phase temperatures. Results: The best results were obtained when using a mobile phase composition of 20% phosphate buffer pH 2.5 or pH 3 and 80% acetonitrile v/v at a flow rate of 2 mL/min at 220 nm. Conclusion: This rapid and easy-to-use HPLC method describes the effect of changing important chromatographic parameters on separation and retention time of cannabinoids and can be effectively applied for high throughput analysis.

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