Special Emphasis on Bioanalytical Method Development and Validation of an Anti-Hypertensive Drug Azelnidipine by LC-ESI-MS/MS in Healthy Human Volunteer’s Blood Plasma

2021 ◽  
pp. 3571-3577
Author(s):  
Dibya Das ◽  
Dhiman Halder ◽  
Himangshu Sekhar Maji ◽  
Pintu Kumar De ◽  
Tapan Kumar Pal
Keyword(s):  
Method Development ◽  
Ammonium Acetate ◽  
Channel Blocker ◽  
Healthy Human ◽  
Bioanalytical Method ◽  
Esi Ms ◽  
Validation Parameters ◽  
Method Development And Validation ◽  
Hypertensive Drug ◽  
Development And Validation

The aim of this study is to develop and validate an accurate, sensitive, rapid, precise, and simple bioanalytical method for the estimation of Azelnidipine (calcium channel blocker, used in hypertension) in the human plasma by using LC-ESI-MS/MS. The method was developed by gradient conditions using 0.1% Formic Acid in Acetonitrile and Milli-Q water with 10mM Ammonium acetate as a mobile phase with a flow rate of 0.5 mL/min. The Analyte and IS (Metoprolol) were separated by using a C18 Phenomenex Kinetex (50x3mm, 5µ) column. 7.0 minutes was the chromatographic run time. The analyte and IS extracted from plasma by simple protein precipitation technique (PPT). The LOD and LLOQ were found to be 0.53125ng/mL and 1.0625ng/mL, respectively. The extraction recovery of the drug from plasma was high. The other validation parameters were found within the range, as mentioned by USFDA and EMA guidelines.

Introduction of an Innovative approach for Bioanalytical Method Development and Validation of Febuxostat by using LC-ESI-MS/MS in Human Plasma

2021 ◽  
pp. 4060-4066
Author(s):  
Dibya Das ◽  
Dhiman Halder ◽  
Himangshu Sekhar Maji ◽  
Pintu Kumar De ◽  
Sudipta Saha ◽  
...  
Keyword(s):  
Formic Acid ◽  
Human Plasma ◽  
Method Development ◽  
Gradient Elution ◽  
Bioanalytical Method ◽  
Esi Ms ◽  
Validation Parameters ◽  
Method Development And Validation ◽  
Development And Validation ◽  
Plasma Extraction

The aim of the present work is to develop and validate an accurate, sensitive, rapid, precise, and simple bioanalytical method for estimation of Febuxostat in human plasma by using LC-ESI-MS/MS. The method was developed by gradient elution technique with the combination of the mobile phase as 0.1% Formic Acid in Milli-Q water and 0.1% Formic Acid in Acetonitrile at a flow rate of 0.5ml/min. The Analyte and IS (Tolbutamide) were separated by a C18 Phenomenex Kinetex (50x3mm, 5µ) column. The chromatographic run time was 7.0 minutes. The plasma extraction was done by a simple protein precipitation technique (PPT). The LOD and LLOQ were found to be 6.25ng/ml and 125ng/ml, respectively. The extraction recovery of the drug from plasma was more than 90%. The validation parameters were found within the range, as mentioned by USFDA and EMA guidelines.

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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