ANALYTICAL METHOD DEVELOPMENT AND VALIDATION STUDIES OF GEMCITABINE NIOSOMES

INDIAN DRUGS ◽  
2021 ◽  
Vol 57 (11) ◽  
pp. 45-51
Author(s):  
Pooja Manjarekar ◽  
Tabassum Khan
Keyword(s):  
Analytical Method ◽  
Validation Studies ◽  
High Performance ◽  
Method Development ◽  
Low Cost ◽  
High Performance Liquid Chromatographic ◽  
Good Resolution ◽  
Mobile Phase Flow Rate ◽  
Gemcitabine Hydrochloride ◽  
Short Run

Gemcitabine hydrochloride niosomes were developed in our laboratory in an effort to improve the efficacy of the drug via development of nanotechnology based delivery system. As a part of this exercise, an analytical method was developed and validated to evaluate the developed formulation for assay and release profile studies. A simple, precise, specific and rapid high performance liquid chromatographic method was developed for determination of gemcitabine hydrochloride in niosomes. The developed method exhibited good resolution, short run time and low cost of analysis. The chromatographic analysis was carried on a Waters® (C18, 250 mm x4.6 mm, 5µ) column using water: acetonitrile (95:5 v/v) as the mobile phase, flow rate of 1.2 ml/min and detection at 268 nm. The robustness of the method was evaluated using design of experiments. The validation studies of the developed method were conducted as per ICH guidelines Q2 (R1). The results indicated that the developed method as specific, accurate, precise, reliable, robust, reproducible, and suitable for the quantitative analysis of gemcitabine hydrochloride in the developed niosomes.

scholarly journals ANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF AMLODIPINE IN HUMAN PLASMA USING LIQUID CHROMATOGRAPHY-MASS SPECTROMETRY/MASS SPECTROMETRY

2018 ◽  
Vol 11 (7) ◽  
pp. 393
Author(s):  
Akiful Haque M ◽  
Shanthi Priya D K ◽  
Dibyalochan Mohanty ◽  
Vasudha Bakshi ◽  
Narender Boggula
Keyword(s):  
Mass Spectrometry ◽  
Human Plasma ◽  
Analytical Method ◽  
High Performance ◽  
Method Development ◽  
Solid Phase ◽  
Internal Standard ◽  
High Performance Liquid Chromatographic ◽  
Economic Method ◽  
Positive Ion

Objective: The objective of the present investigation was to develop a novel, simple, and economic method for the estimation of amlodipine in positive ion mode in human plasma using amlodipine maleate d4 as an internal standard.Methods: The chromatographic separation was performed on Zorbax SB, C18, 50 mm*4.6 mm, and 3.5 mm. The mobile phase was prepared with a mixture of 5 mm ammonium acetate in 0.1% formic acid: High performance liquid chromatographic (HPLC) grade methanol:HPLC grade acetonitrile (40:30:30) that run isocratically at the flow rate of 0.700 ml/min and run time at 2.50 min.Results: The analytical method is valid for the estimation of amlodipine, in human plasma over a range of 0.100 ng/ml–9.990 ng/ml with the detection of amlodipine m/z - 409.10 (parent) and 238.00 (product), and internal standard Amlodipine Maleate d4 m/z - 413.20 (parent), and 238.00 (product) in positive ion mode. The results of carryover test, matrix effect, linearity, precision and accuracy, stabilities, dilution integrity, and run size evaluation test presented in this report are within the acceptance range.Conclusion: A sensitive method for the separation and determination of amlodipine in plasma has been developed based on solid-phase extraction with disposable extraction cartridges in combination with LC and mass spectrophotometers (MS/MS).

scholarly journals RP-HPLC method development and validation for simultaneous estimation of Cilnidipine, Atenolol and Chlorthalidone

2018 ◽  
Vol 8 (6-s) ◽  
pp. 78-82 ◽  
Author(s):  
Vishal Singh Solanki ◽  
RAM SINGH BISHNOI ◽  
Raviraj Baghel ◽  
Deepti Jain
Keyword(s):  
High Performance ◽  
Chromatographic Method ◽  
Method Development ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Good Resolution ◽  
Rp Hplc ◽  
Tablet Dosage ◽  
Liquid Chromatographic

A simple precise and economical reverse phase high performance liquid chromatographic method has been developed and validated for the simultaneous estimation of Cilnidipine (CDP), Atenolol (ATL) and Chlorthalidone (CTD).The chromatographic separation was achieved by using Hypersil- keystone C18 (4.6 x 250mm, 5μm) under isocratic conditions The mobile phase consisted of methanol and triple distilled water (80/20, v/v) having pH 7 with a flow rate of 1.0 mL/min. The eluents were monitored at 225 nm for simultaneous measurement.The selected chromatographic conditions were found to effectively separate CDP (Rt: 3.25 min), ATL (Rt: 5.366 min) and CTD (Rt: 9.025 min) having good resolution. The developed method was validated for linearity, accuracy, precision, LOD, LOQ, robustness and for system suitability parameters as per ICH guidelines. In this study, an excellent linearity was obtained with r2 = 0.999, r² = 0.999, r² = 1, for CDP, ATL and CTD respectively. The developed chromatographic method proved to be simple, precise, accurate, robust and reproducible Thus, this method would be employed for routine simultaneous quantification of CDP, ATL and CTD in bulk form or tablet dosage form.   Keywords: Cilnidipine, Atenolol and Chlorthalidone, RP-HPLC.

scholarly journals METHOD DEVELOPMENT, VALIDATION AND STABILITY STUDIES FOR THE DETERMINATION OF LURASIDONE HYDROCHLORIDE IN BULK AND TABLET DOSAGE FORM BY RP-HPLC

2018 ◽  
Vol 10 (12) ◽  
pp. 58
Author(s):  
Bhavani Thota ◽  
Geetha Susmita Adepu ◽  
Rajitha Galla
Keyword(s):  
High Performance ◽  
Method Development ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Control Analysis ◽  
Mobile Phase Flow Rate ◽  
Rp Hplc ◽  
Degradation Studies ◽  
Tablet Dosage ◽  
Lurasidone Hydrochloride

Objective:  To  develop  a  simple,  rapid,  sensitive,  precise,  accurate,  economical  and  validated reverse  phase  high  performance  liquid  chromatographic  (RP-HPLC)  method  for  the  estimation  of lurasidone hydrochloride in tablet dosage form.Methods:    The  chromatographic  separation  was  carried  out  on  a  prontosil  C18,  AQ  (100 mm×4.6mm,  3µm)  column.  A mixture of phosphate buffer (pH 3.0): acetonitrile (ACN) (55:45v/v) was used as a mobile phase. Flow rate of 1.0 ml/min and 10 μl injection volume was used for the assay.  PDA detector was used and the detection wavelength was 230 nm.  The retention time (RT) of lurasidone hydrochloride was found to be 4.505 ± 0.01 min. The method was validated according to the ICH guidelines.Results:   The   calibration   curve   for   lurasidone   hydrochloride   was   linear   with   correlation coefficient value 0.999 in the concentration range of 25-125%. Specificity, accuracy (% mean recovery, 99.08%), precision, detection limits, robustness (%RSD˂2) and system suitability were found to be within the limits.  Degradation studies were performed under different stressed conditions and the results of degradation studies reveals that the developed method was stable.Conclusion:   The developed method was simple, reliable, economical and stable and it can be applied  for  the  routine  quality  control  analysis  of  lurasidone hydrochloride  in  tablet  dosage forms. 

scholarly journals METHOD DEVELOPMENT AND VALIDATION FOR ESTIMATION OF MELATONIN IN TABLET BY USING RP-HPLC

2021 ◽  
Vol 11 (6) ◽  
pp. 54-61
Author(s):  
Khanderao Rajaram Jadhav
Keyword(s):  
High Performance ◽  
Method Development ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Good Precision ◽  
Good Resolution ◽  
Uv Detector ◽  
Rp Hplc ◽  
Liquid Chromatographic

In the present work new, Simple Reversed-Phase High Performance Liquid Chromatographic method was developed and validated for the estimation of Melatonin in tablets. A sharp peak was obtained 7.125 min using Methanol: Phosphate buffer (PH 3.0) in the ratio of 40:60 as mobile phase at a flow rate of 1.0 ml/min, on HPLC Waters 515 system containing UV detector with Empower software. The separation was achieved on the C18 analytical column (250 mm × 4.6 mm, 5.0 μm). The detection was carried out at 223 nm. The method gave good resolution and suitable retention time. The results of the analysis in this method were validated in terms of specificity, accuracy, precision, linearity, and range. The method was found to be reliable, reproducible, rapid, and economic. The RP-HPLC method developed in this study showed specificity and selectivity with linearity in the working range and good precision and accuracy, making it very suitable for the estimation of Melatonin in tablets.

Method Development and Validation of Propofol by Reverse Phase HPLC and its Estimation in Commercial Formulation

2021 ◽  
pp. 3139-3142
Author(s):  
Kuntal Mukherjee ◽  
S. T. Narenderan ◽  
B. Babu ◽  
Survi Mishra ◽  
S. N. Meyyanathan
Keyword(s):  
High Performance ◽  
Method Development ◽  
Pharmaceutical Formulations ◽  
High Performance Liquid Chromatographic ◽  
Reverse Phase Hplc ◽  
Liquid Chromatographic Method ◽  
Method Development And Validation ◽  
Development And Validation ◽  
Liquid Chromatographic

A simple, sensitive and rapid high performance liquid chromatographic method has been developed for the determination of Propofol. The main focus of the method was to determine Propofol in solution form as well as in marketed formulation. Chromatographic separation was achieved on Inertsil ODS-3V column (250mm x 4.6mm; 5µm) with a mobile phase consisting of methanol: water (85:15), with a flow rate of 1.0ml/min (UV detection at 270nm). Linearity was observed over the concentration range of 10-110µg/ml with a regression equation y=88048x + 44524 and having a regression value (R2) of 0.999. The LOD and LOQ values found to be 10ng and 100ng, respectively. No changes found in ruggedness and robustness studies. The percentage of recovery was found to be 95.25% to 101.81%. Validation studies revealed that the method was specific, accurate, precise, reliable, robust, reproducible and suitable for the quantitative analysis in its pharmaceutical formulations.

scholarly journals Method Development and Validation of Metoprolol and Felodipine by using RP-HPLC in Bulk and Pharmaceutical Dosage Form

2020 ◽  
Vol 11 (4) ◽  
pp. 8047-8053
Author(s):  
Potturi Ramadevi ◽  
Kantipudi Rambabu
Keyword(s):  
High Performance ◽  
Method Development ◽  
Pharmaceutical Preparations ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Concentration Limit ◽  
Uv Detector ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc

The main objective of this research is to develop and validate a simple, specific, precise, sensitive, cost effective and rapid Reversed-Phase High-Performance Liquid Chromatographic (RP-HPLC) method for simultaneous quantification of Felodipine and Metoprolol in bulk and pharmaceutical dosage forms. The separation of the analytes were carried out on a X-bridge phenyl column with a moving phase composed of 0.1 % Tri ethyl amine: acetonitrile (30:70 v/v) delivered at a stream of 1.0 ml/min, and separation has been observed by UV detector, at a detection wavelength of 235 nm. This method was proven to be linear over a concentration limit of 10-150 µg/ml for Metoprolol, 2-30 µg/ml for Felodipine with correlation coefficient of 0.999. The retention time of Metoprolol and Felodipine were 2.936, 4.535 minutes respectively. To separate Metoprolol and Felodipine peaks a run time of 8 min. was used. The validation results were in good agreement with acceptable limits. RSD values which are less than 2.0 % indicating the accuracy and precision of this method. Hence it was evident that the proposed method was said to be a suitable one for the regular analysis and quality control of pharmaceutical preparations which contain these active drugs either individually or in combination.

ANALYTICAL METHOD DEVELOPMENT AND VALIDATION FOR THE SIMULTANEOUS ESTIMATION OF ABACAVIR SULPHATE AND LAMIVUDINE IN TABLET DOSAGE FORM BY RP-HPLC

INDIAN DRUGS ◽  
2015 ◽  
Vol 52 (08) ◽  
pp. 12-16
Author(s):  
S Vidyadhara ◽  
◽  
L. S Reddyvalam ◽  
T. Koduri ◽  
P. K. Borra ◽  
...  
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
Method Development ◽  
Correlation Coefficients ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Development And Validation ◽  
Tablet Dosage ◽  
Liquid Chromatographic

A simple, accurate, precise high-performance liquid chromatographic (HPLC) method has been developed and validated for the simultaneous determination of abacavir sulphate (ABA) and lamivudine (LAM) in combined dosage form. Separation was performed on a C18 column [Agilent ODS UG 5 column, 250 mm x 4.5 mm], with methanol: water (50:50 V/V) isocratic elution using a flow rate of 1mL/min. Good sensitivity was observed with UV detection at 277 nm. After method development, the interference of other active compounds and excipients, repeatability and linearity, were investigated. Retention times of LAM and ABA were found to be 3.3 and 6.3 min, respectively. The method was validated over the range from 2.5-12.5 μg/mL for LAM and 5-25 μg/mL for ABA with correlation coefficients of 0.9997 and 0.9996, respectively. This method was shown to be accurate, robust, selective, linear, and repeatable and can be successfully employed in routine quality control for the simultaneous analysis of ABA and LAM in tablets.

scholarly journals ANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF ATOMOXETINE HYDROCHLORIDE USING RAPID HIGH-PERFORMANCE LIQUID CHROMATOGRAPHIC TECHNIQUE

2018 ◽  
Vol 11 (11) ◽  
pp. 118
Author(s):  
Zubaidur Rahman ◽  
Vijey Aanandhi M ◽  
Sumithra M
Keyword(s):  
High Performance ◽  
Method Development ◽  
High Sensitivity ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Chromatographic Technique ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc ◽  
Liquid Chromatographic

Objective: A simple, novel, sensitive, rapid high-performance liquid chromatographic (RP-HPLC) method has been developed and validated for quantitative determination of atomoxetine HCl (ATH) in bulk and formulations.Methods: The chromatographic development was carried out on RP-HPLC. The column used as Xterra RP 18 (250 mm × 4.6 mm, 5 μ particle size), with mobile phase consisting of methanol: water 80:20 V/V. The flow rate was 1.0 mL/min and the effluents were monitored at 270 nm.Results: The retention time was found to be 5.350 min. The method was validated as per International Conference on Harmonization Guideline with respect to linearity, accuracy, precision, and robustness. The calibration curve was found to be linear over a range of 2–10 μg/mL with a regression coefficient of 0.9999. The method has proved high sensitivity and specificity.Conclusion: The results of the study showed that the proposed RP-HPLC method was simple, rapid, precise and accurate which is useful for the routine determination of ATH in bulk drug and in its pharmaceutical dosage form.

scholarly journals Stability-Indicating High-Performance Liquid Chromatographic Assay of Atorvastatin with Fluorescence Detection

2007 ◽  
Vol 90 (6) ◽  
pp. 1547-1553 ◽  
Author(s):  
Alaa Khedr
Keyword(s):  
High Performance ◽  
Uv Light ◽  
Degradation Products ◽  
High Performance Liquid Chromatographic ◽  
Base Hydrolysis ◽  
Good Resolution ◽  
Stability Indicating ◽  
Limit Of Quantitation ◽  
Bulk Drug ◽  
Liquid Chromatographic

Abstract The purpose of this work was to develop a sensitive, selective, and validated stability-indicating high-performance liquid chromatographic (LC) assay of atorvastatin (ATV) in bulk drug and tablet form. ATV was subjected to different stress conditions, including UV light, oxidation, acid-base hydrolysis, and temperature. ATV and its degradation products were analyzed on an Agilent Zorbax XDB C18 column using isocratic elution with acetonitrile0.02 M sodium acetate, pH 4.2 (45 + 55, v/v) for 25 min. The samples were monitored with fluorescence (FL) detection at 282 nm (excitation)/400 nm (emission). The response ratio of FL to UV detection (at 247 nm) for ATV was 1.66. The method showed good resolution of ATV from its decomposition products. The photodegradation products were separated by silica gel thin-layer chromatography using double development with ethyl acetaten-hexaneglacial acetic acidmethanol (40 + 55 + 0.5 + 4.5, v/v/v/v) followed by (39 + 55 + 0.5 + 5.5, v/v/v/v), and confirmed by LC-FL analysis. The FL response was linear over the investigated range for ATV. The linear range was 101200 ng/injection, and the limit of quantitation was 2.0 ng/injection.

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