scholarly journals Stability Indicating HPLC Method for Estimation of Thymoquinone in Nasal Simulated Fluid: Method Development and Validation

2021 ◽  
pp. 233-240
Author(s):  
Sagar Trivedi ◽  
Abhidha Deshpande ◽  
Veena Belgamwar ◽  
Vidyadevi Bhoyar ◽  
Kamlesh Wadher
Keyword(s):  
Method Development ◽  
Degradation Products ◽  
Hplc Method ◽  
Stress Studies ◽  
Specificity And Sensitivity ◽  
Accuracy And Precision ◽  
Validation Parameters ◽  
Quality Control Tool ◽  
Method Development And Validation ◽  
Development And Validation

Introduction: A simple rapid and precise HPLC method was developed for estimation of TH in nasal simulated fluid and stability was assessed in various stressed conditions. Methods: Chromatographic separation of TH in nasal simulated fluid was done using HPLC AS-4050 coupled with Jasco UV 2075 Plus detector, Jasco LC-Net 11/ADC valve, Jasco PU-2080 pump and hypersil gold C18 (250x6x5 µm) column, ChromNAV 2.0 Chromatography Data System software with mobile phase as acetonitrile: water (65:35) and acetonitrile: NSF (60:40) at a flow rate of 1ml/min and having run time of 10 min with loop volume of 20 µl and detection wavelength of 252 nm. The method was validated for accuracy, precision, linearity, specificity, and sensitivity in accordance with ICH (Q2B) guidelines. Results: The results of all the validation parameters were found to be within the acceptable limits. The calibration plots were linear over the concentration ranges from 2 to 14µg/ml. The accuracy and precision were found to be between 97.04±0.112 to101.081±0.0191and ≤2% for three drugs. Developed method was successfully applied for the determination TH in nasal simulated fluid and recovery was found to be >98% for three drugs. The degradation products produced as a result of stress studies did not interfere with drug peak. Conclusion: The developed method was found to be simple, specific, economic, reliable, accurate, precise, and reproducible used as a quality control tool for analysis of pure thymoquinone in nasal simulated fluid.

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.

scholarly journals A New Quantitative Analytical Method Development and Validation for the Analysis of Boceprevir in Bulk and Marketed Formulation

2018 ◽  
Vol 10 (03) ◽  
Author(s):  
Bhetanabotla Chandramowli ◽  
B.M Syam Kumar ◽  
D.V. R. N. Bhikshapathi ◽  
Bigala B Rajkamal
Keyword(s):  
Chromatographic Analysis ◽  
Mobile Phase ◽  
Method Development ◽  
Hplc Method ◽  
Capsule Formulation ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Validation Parameters ◽  
Method Development And Validation ◽  
Development And Validation

A simple, precise and accurate RP-HPLC technique was developed and the developed method was validated for the regular analysis of Boceprevir. Chromatographic analysis was performed by selecting X-Terra ODS ( C18) column (4.6 mm i.d. × 250 mm, 5μ), Acetonitrile : Phosphate buffer pH -3 ( 90 : 10% v/v) as mobile phase, 1.0 ml/min as flow rate and 20μl injection volume. The LC chromatographic peak was eluted at 3.6 min at 235 nm as UV detection wavelength. The developed method was validated as per the ICH guidelines and the Validation parameters were specificity, accuracy, linearity, precision, LOD and LOQ. Linear relationship for Boceprevir established in the concentration range of 50 to 150μg/mL. Accuracy in terms of percentage recovery found in the range between 98 to 101%. LOD and LOQ values were found to be 2.3 and 7.123μg/mL respectively. The results of the method established that the new RP-HPLC method is convenient and simple in regular analysis of Boceprevir in bulk and capsule formulation.

Bioanalytical Method Development and Validation for the Determination of Vasopressin Receptor Antagonist Conivaptan in Mouse Plasma at NanoLevel and its Pharmacokinetic Application

2019 ◽  
Vol 15 (5) ◽  
pp. 591-598 ◽  
Author(s):  
Haitham Alrabiah ◽  
Ahmed Bakheit ◽  
Sabray Attia ◽  
Gamal A.E. Mostafa
Keyword(s):  
Method Development ◽  
Internal Standard ◽  
Vasopressin Receptor ◽  
Mouse Plasma ◽  
Precipitation Procedure ◽  
Validation Parameters ◽  
The Us ◽  
Method Development And Validation ◽  
Development And Validation

Background: Conivaptan inhibits two of vasopressin receptor (vasopressin receptor V1a and V2). Conivaptan is used for the treatment of hyponatremia, and in some instances, for the treatment of the heart failure. Methods: The present study aimed to develop a simple, sensitive, and accurate HPLC with ultraviolet detection for the assay of conivaptan (CON) in mouse plasma using bisoprolol as internal standard (IS). A precipitation procedure was used to extract CON and the IS from the mouse plasma. CON was chromatographically separated using a C18 analytical column at 25°C. The separation was carried out using a mixture of phosphate buffer (50 mM): acetonitrile (60: 40, v/v, pH 4.5) with a flow rate of 1.0 mL/min and detection was performed at 240 nm. Results: The assay was validated according to the US Food and Drug (FDA) guidelines. The method demonstrated linearity over a concentration range of 150 - 2000 ng/mL (correlation coefficient: r 2 = 0.9985). The mean recovery of CON from the mouse plasma was 101.13%. All validation parameters for CON were within the acceptable range. Conclusion: The investigated method has been shown to be suitable for estimating the CON in plasma samples, and this method is sensitive and highly selective, allowing the estimation of its concentrations up to the nano-scale. The suggested method was successfully used in a pharmacokinetic study of CON in mouse plasma.

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