A NEW METHOD DEVELOPMENT AND VALIDATION FOR RELATED SUBSTANCES OF GRANISETRON IN ACTIVE PHARMA INGREDIENT BY HPLC

INDIAN DRUGS ◽  
2017 ◽  
Vol 54 (07) ◽  
pp. 52-59
Author(s):  
T. N Rao ◽  
◽  
Y. Prasanthi ◽  
Parvatamma Botsa ◽  
G. Kumara ◽  
...  
Keyword(s):  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Limit Of Quantification ◽  
Chromatographic Separations ◽  
Column Temperature ◽  
Related Substances ◽  
System Suitability ◽  
Method Development And Validation ◽  
Development And Validation

A simple and inexpensive method was developed using high performance liquid chromatography with PDA detection for determination of granisetron hydrochloride and related impurities (2-methyl-N- [(1R,3r,5S)-9-methyl-9-azabicyclo[3.3.1]non-3-yl]-2H-indazole-3-carboxamide, 1-Methyl-N-[(1R,3r,5S)- 9-methyl-9-azabicyclo[3.3.1]non-3-yl]-1H-indazole-3-carboxamide hydrochloride, N-[(1R,3r,5S)-9- azabicyclo[3.3.1]non-3-yl]-1-methyl-1H-indazole-3-carboxamide and 1-methyl-1H-indazole-3-carboxylic acid. The chromatographic separations were achieved on (250×4.6 mm), 5.0 μm make: Waters, Symmetry Shield C8 column employing acetonitrile: 2% V/V H3PO4 in MilliQ water + 0.1% V/V hexylamine in water, 800:200 V/V (pH adjusted to 7.5 using triethylamine) mobile phase with isocratic programme. A flow rate of 1.5 mL/min was chosen. Four impurities were eluted within 20 minutes. The column temperature was maintained at 40°C and a detector wavelength of 300 nm was employed. The method was successfully validated by establishing system suitability, specificity, linearity, accuracy, limit of detection and limit of quantification.

scholarly journals Method Development and Validation of Metformin Hydrochloride in Tablet Dosage Form

2011 ◽  
Vol 8 (3) ◽  
pp. 1309-1313 ◽  
Author(s):  
Kaushelendra Mishra ◽  
Himesh Soni ◽  
Govind Nayak ◽  
Sita Sharan Patel ◽  
A. K. Singhai
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Wave Length ◽  
Metformin Hydrochloride ◽  
Limit Of Quantification ◽  
System Suitability ◽  
Method Development And Validation ◽  
Development And Validation ◽  
Tablet Dosage

A simple, reproducible and efficient method for the determination of metformin hydrochloride (MET) was developed and validated. The analysis complied with Beer's law in the concentration range of 8-13 μg/mL at 233 nm for MET. In our study the validation of analytical method for determination of MET by UV in tablets formulation was performed in accordance the parameters including-system suitability, specificity, limit of quantification, limit of detection, linearity of response, accuracy, precision (reproducibility & repeatability), robustness (change of wave length±2 nm).

ANALYTICAL METHOD DEVELOPMENT AND VALIDATION FOR ESTIMATION OF APIXABAN BY RP-HPLC

INDIAN DRUGS ◽  
2017 ◽  
Vol 54 (04) ◽  
pp. 76-79
Author(s):  
A. M Kashid ◽  
M. B. Vidhate ◽  
M. R Ingale ◽  
Keyword(s):  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Standard Addition ◽  
High Performance Liquid Chromatographic ◽  
Limit Of Quantification ◽  
Liquid Chromatographic Method ◽  
Method Development And Validation ◽  
Development And Validation ◽  
Liquid Chromatographic

A simple, fast and precise high performance liquid chromatographic method is developed and validated for apixaban as per ICH guideline. Chromatographic separation of drugs was performed on a Kromasil C18 column (250 mm x 4.6 mm, 5 μ) with a mobile phase comprising of sodium acetate: acetonitrile in the ratio 50:50 (V/V) at a flow rate of 1 mL/min. The described method was linear over a concentration range of 10-50μg/mL (r2> 0.994) for apixaban. The limit of detection (LOD) was found to be 0.36μg/mL, whereas the limit of quantification (LOQ) was found to be 1.09μg/mL. The recovery was calculated by the standard addition method. The average recovery was found to be 96.87 %. Developed method was found to be simple, accurate, precise and rapid, hence it can be used for quality control of apixaban.

High performance liquid chromatography (HPLC) method development and validation for the determination of flunixin: Animal plasma based study

2021 ◽  
pp. 1-11
Author(s):  
Sultan M. Alshahrani ◽  
John Mark Christensen
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Mobile Phases ◽  
Hplc Method Development ◽  
Development And Validation

This study was designed to develop and validate a simple and efficient high performance liquid chromatography (HPLC) method to determine flunixin concentrations in Asian elephant’s (Elephas maximus) plasma. Flunixin was administered orally at a dose of 0.8 mg/kg, and blood samples were collected. Flunixin extraction was performed by adding an equal amount of acetonitrile to plasma and centrifuging at 4500 rpm for 25 minutes. The supernatant was removed, and flunixin was analyzed using HPLC-UV detection. Two methods were developed and tested utilizing two different mobile phases either with or without adding methanol (ACN: H2O vs. ACN: H2O: MeOH). Both methods showed excellent linearity and reproducibility. The limit of detection was 0.05 ug/ml and limit of quantification was 0.1 ug/ml. the efficiency of flunixin recovery was maximized by the addition of methanol to mobile phase (ACN: H2O: MeOH as 50:30:20) at 95% in comparison to 23% without methanol. In conclusion, adding methanol to HPLC methods for extraction of flunixin from elephants’ plasma yielded higher recovery rate than without methanol.

scholarly journals Analytical Method Development and Validation of Rp-Hplc Method for Simultaneous Estimation of Pyridoxamine Dihydrochloride and Acetylcysteine in Tablet Dosage Form.

2021 ◽  
Vol 23 (06) ◽  
pp. 992-1000
Author(s):  
Sneha S. Ghule ◽  
◽  
Ashpak M. Tamboli ◽  
Snehal D. Patil ◽  
◽  
...  
Keyword(s):  
High Performance ◽  
Method Development ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Rp Hplc ◽  
System Suitability ◽  
Validation Parameters ◽  
Method Development And Validation ◽  
Development And Validation ◽  
Tablet Dosage

A reverse-phase high-performance liquid chromatography (RP-HPLC) method for the simultaneous estimation of Pyridoxamine dihydrochloride and Acetylcysteine in the marketed formulation is developed. Chromatography carried out at 30oc temperature on Agilent Zorbax Bonus-RP (250 x 4.6 mm, 5 µ) coloum. Coloum using a mobile phase 0.1% trifluroacetic acid in water: acetonitrile (80:20v/v) with flow rate 1ml/min (DAD scan at 210nm). Validation parameters such as system suitability, linearity, precision, accuracy are considered as reported International Conference on Harmonization guidelines. The retention times for Pyridoxamine dihydrochloride and Acetylcysteine are 2 min and 3.4 min. The linearity range for Pyridoxamine dihydrochloride and Acetylcysteine is 30-70 µg/ml and 180-420 µg/ml. The %RSD for accuracy was found to be less than 2%. Hence the proposed method was found to be accurate, precise, reproducible, and specific and can be used for simultaneous analysis of these drugs in tablet formulation.

METHOD DEVELOPMENT AND VALIDATION FOR THE SIMULTANEOUS ESTIMATION OF THYMOL AND EUGENOL BY USING RP-HPLC IN PURE AND IN EMULGEL FORMULATION

INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (07) ◽  
pp. 59-65
Author(s):  
Vinita C. Patole ◽  
Shilpa P. Chaudhari ◽  
Keyword(s):  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Peak Areas ◽  
80 A 20 ◽  
Development And Validation

An attempt was made to develop a simple, selective, rapid and precise high-performance liquid chromatography (HPLC) method for simultaneous estimation of thymol and eugenol. Analysis was performed on a C18 column with the mobile phase consisting of solvent %A (water) and solvent %B (acetonitrile) with the following gradient: 0–1 min, 80 % A, 20 % B; 1–7 min, 40 % A and 60 % B; 7–12 min, 10 % A and 90 % B; and 12–15min, 80 % A and 20 % B at a flow rate of 0.6 mL/min. The compounds were well separated on a Thermo Scientific Hypersil BDS RP C18 column (4.6 mm × 150 mm, dp = 5 µm) and ultraviolet detection at 280 nm. The retention times of eugenol and thymol were 10.5 min and 11.6 min, respectively. Validation of the proposed method was carried out according to the guidelines of the International Council on Harmonization (ICH). The linearity of the method is good for thymol and eugenol over the concentration range of 1–50 ppm, and the r 2 values were 0.9996 for both thymol and eugenol. The calculated limit of detection (LOD) value was 0.5ppm and the limit of quantification (LOQ) value was 1ppm for both the analytes. The intra and interday relative standard deviation (RSD) of the retention time and peak areas was less than 3 %.The established method was appropriate, and the two markers were well resolved, enabling efficient quantitative analysis of thymol and eugenol.

Simultaneous Determination of Cholecalciferol and 25- Hydroxycholecalceferol in Lipid-based Self-nanoemulsifying formulations and Marketed Product Vi-de 3® by UHPLC-UV

2019 ◽  
Vol 16 (1) ◽  
pp. 100-109
Author(s):  
Ibrahim Aljuffali ◽  
Fahad Almarri ◽  
A. F. M. Motiur Rahman ◽  
Fars Kaed Alanazi ◽  
Musaed Alkholief ◽  
...  
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Simultaneous Estimation ◽  
Limit Of Quantification ◽  
Column Temperature ◽  
Related Substances ◽  
Accuracy And Precision ◽  
Regulatory Guidelines ◽  
25 Hydroxycholecalciferol

Background: The purpose of the current study was to develop a selective, precise, fast economical and advanced reverse phase ultra-high-performance liquid chromatography (UHPLC UV) method and validate it for the simultaneous estimation of cholecalciferol and its analogue 25- hydroxycholecalciferol in lipid-based self-nano emulsifying formulation (SNEDDS). Methods: The chromatographic separation was simply performed on a Dionex® UHPLC systems (Ultimate 3000, Thermo scientific) by using HSS C18 (2.1x50 mm, 1.8 µm) analytical column. The elution was carried out isocratically with the mobile phase consisting of acetonitrile and methanol in the ratio of 50:50 %v/v with a flow rate of 0.4 ml/min, followed by the UV detection at 265 nm. The injection volume was 1µl and the column temperature was maintained at 45°C. FDA regulatory guidelines were used to develop and validate the method. Results: The current developed UHPLC-UV method was found to be rapid (run time 2 min), and selective with the high resolution of cholecalciferol and 25-hydroxycholecalciferol (RT=0.530 min & 1.360 min) from different lipid matrices. The method was highly sensitive (Limit of Detection and Lower Limit of Quantification were 0.13 ppm & 0.51ppm, and 0.15 ppm & 0.54 ppm, respectively). The linearity, accuracy and precision were determined as suitable over the concentration range of 0.5-50.0 ppm for both the analytes. Conclusion: The proposed UHPLC-UV method can be used for the determination of cholecalciferol and 25-hydroxycholecalciferol in SNEDDS and marketed Vi-De 3® as pure forms (intact) with no interference of excipients or drug-related substances.

Key Aspects of Analytical Method Development and Validation

2019 ◽  
Vol 31 (1) ◽  
pp. 32-39
Author(s):  
Suman Shrivastava ◽  
Pooja Deshpande ◽  
S. J. Daharwal
Keyword(s):  
Method Validation ◽  
Analytical Method ◽  
Method Development ◽  
Limit Of Detection ◽  
Limit Of Quantification ◽  
Ich Guidelines ◽  
Validation Parameters ◽  
Method Development And Validation ◽  
Key Aspects ◽  
Development And Validation

Development of a method is crucial for discovery, development, and analysis of medicines in the pharmaceutical formulation. Method validation could also be thought to be one in all the foremost well-known areas in analytical chemistry as is reproduced within the substantial variety of articles submitted and presented in peer review journals every year. Validation of an analytical procedure is to demonstrate that it's appropriate for its intended purpose. Results from method validation are often wont to decide the quality, reliability and consistency of analytical results. Analytical methods need to be validated or revalidated. This review describes general approach towards validation process and validation parameters to be considered during validation of an analytical method. It also refers to various regulatory requirements like WHO, USFDA, EMEA, ICH, ISO/IEC. The parameters described here are according to ICH guidelines which include accuracy, precision, specificity, limit of detection, limit of quantification, linearity range and robustness.

A REVIEW ON METHOD DEVELOPMENT AND VALIDATION BY USING HPLC

2021 ◽  
pp. 34-37
Author(s):  
Dipali S. Doifode ◽  
Shailesh G. Jawarkar ◽  
Monika P. Jadhao ◽  
Manali M. Bode
Keyword(s):  
Quality Assurance ◽  
Analytical Method ◽  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Science Research ◽  
Hplc Method ◽  
Pharmaceutical Drugs ◽  
Method Development And Validation ◽  
Development And Validation

Analytical method development and validation are the continuous and inter-dependent task associated with the research and development, quality control and quality assurance departments. High performance liquid chromatography (HPLC) has been widely used for years as an analytical method and is a key tool for the separation and analysis of pharmaceutical drugs, for drug monitoring and for quality assurance and life science research. Most of the drugs in multi component dosage forms can be analysed by HPLC method because of the several advantages like rapidity, specicity, accuracy, precision and ease of automation in this method. HPLC methods development and validation play important roles in new discovery, development, manufacture of pharmaceutical drugs and various other studies related to humans and animals. This review gives information regarding principle, types, instrumentation and along with various application of the method and Validation of HPLC method as per ICH Guidelines covers all the performance characteristics of validation, like Accuracy, precision, specicity, linearity, range and limit of detection, limit of quantication, robustness

scholarly journals METHOD DEVELOPMENT AND VALIDATION OF EPROSARTAN MESYLATE AND ITS IMPURITIES USING REVERSE PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY

2016 ◽  
Vol 8 (4) ◽  
pp. 49 ◽  
Author(s):  
O. S. S. Chandana ◽  
D. Sathis Kumar ◽  
R. Ravichandra Babu
Keyword(s):  
High Performance ◽  
Method Development ◽  
Hplc Method ◽  
Reverse Phase ◽  
Related Substances ◽  
Rp Hplc ◽  
Method Development And Validation ◽  
The Mean ◽  
Development And Validation

Objective: Our main objective is to develop an accurate and precise RP-HPLC method for the determination of Eprosartan Mesylate and its impurities. Methods: A Develosil ODS UG-5; (150 × 4.6) mm; 5 µm column was used for the Separation of drugs by a mobile phase consisting of Buffer and Acetonitrile mixture in the gradient proportion. The flow rate maintained was 0.8 ml/min and the wavelength used for detection was 235 nm.Results: The linearity was observed in the range of 0.025-50µg/ml of spiked impurities in Eprosartan Mesylate, impurity 1 and impurity 2 with a correlation coefficient of 0.99927, 0.99910 and 0.99934 respectively. The mean percentage recoveries for LOQ, 50%, 80%, 100%, 150% and 200% accuracy were found to be 101.5±1.51, 107.0±1.7, 104.6±0.4, 102.8±0.36, 101.7±0.26 and 101.3±0.15 respectively for impurities in Eprosartan Mesylate, impurity 1 and impurity 2. Linearity, accuracy, precision and robustness parameters for the suggested method were estimated for validation.Conclusion: The developed method is uncomplicated, accurate, sensitive and precise for the determination of related substances in the Eprosartan Mesylate. The satisfying % recoveries and low % RSD Values confirmed the suitability of the developed method for the usual analysis of Eprosartan mesylate in pharmaceuticals.

scholarly journals HPLC-MS method development and validation for simultaneous quantitation of GZK-111 and CPG compounds in rat plasma

2020 ◽  
pp. 28-36
Author(s):  
A. L. Podolko ◽  
P. O. Bochkov ◽  
G. B. Kolyvanov ◽  
A. A. Litvin ◽  
O. G. Gribakina ◽  
...  
Keyword(s):  
Blood Plasma ◽  
Lower Limit ◽  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Rat Plasma ◽  
Rat Blood ◽  
Method Development And Validation ◽  
Development And Validation

The technique of quantitative determination of GZK-111 and CPG compounds in rat blood plasma has been developed. The analysis was carried out using the combined method of high-performance liquid chromatography with mass spectrometric detection. The method was linear in the concentration range of 25-1000 ng/ml for both compounds. Percentage of GZK-111 extraction from rat blood plasma was 57.8 %. The lower limit of detection for GZK- 111 compound was 25 ng/ml. Percentage of extraction of CPG compound was 42.5 %. The lower limit of detection of CPG compound was also 25 ng/ml.

Sign in / Sign up

Export Citation Format

Share Document