Method development and validation procedure for the chromatographic assay of cocaine and its metabolites in pharmacokinetic studies

1993 ◽  
Vol 36 (1) ◽  
pp. 368-372 ◽  
Author(s):  
L. Tamisier-Karolak ◽  
M. Tod ◽  
O. Petitjean ◽  
Ph. J. P. Cardot
Keyword(s):  
Method Development ◽  
Pharmacokinetic Studies ◽  
Validation Procedure ◽  
Method Development And Validation ◽  
Development And Validation

scholarly journals Bio analytical method development and validation for Ezetimibe and Pitavastain and its applications to pharmacokinetic studies in Rabbit plasma by using LCMS/MS

2020 ◽  
Vol 11 (4) ◽  
pp. 7854-7862
Author(s):  
Potturi Ramadevi ◽  
Kantipudi Rambabu
Keyword(s):  
Method Development ◽  
Extraction Process ◽  
Pharmacokinetic Studies ◽  
Rabbit Plasma ◽  
Highly Sensitive ◽  
The Us ◽  
Positive Mode ◽  
Method Development And Validation ◽  
Development And Validation ◽  
Preparation Techniques

For the gradation of Ezetimibe and Pitavastain in rabbit plasma, a highly sensitive and simple LC-MS/MS assay was developed and witnessed. The chromatographic conditions are isocratic with a waters symmetry C18 (150 x 4.6 mm, 3.5) column in isocratic mode. The detection was carried out using a mobile phase of 0.1 percent formic acid and 60:40 acetonitrile, and the detection was carried out using MS in a positive mode of electrospray ionisation. The valid approach was checked with a linear range of 10-200 ng/ml Ezetimibe and 2-40 ng/ml Pitavastain. The intraday and interday precision values were found to be within reasonable limits. The liquid extraction process is used to remove these drugs from rabbit plasma. And these drugs have been shown to be stable in freeze-thaw, autosampler, and benchtop tests in the future. The fluid chromatography coupled mass spectrometry strategy was approved by the US Food and Drug Administration for quantification of Ezetimibe and Pitavastain in rabbit plasma using D4–ezetimibe and D4–pitavastain as within norms using LC-MS consolidated with quadrupole spectrometer by electro shower ionisation process. The aim of this study is to evaluate the applicability of this approach to ezetimibe and pitavastain at different evaluation levels while taking into account various factors such as instrument stability, precision, and accuracy, sample preparation techniques, instrument calibration, recovery, and matrix effect by using Ezetimibe and Pitavastain, as well as their internal guidelines.

Bioanalytical Method Development and Validation of Naproxen: Application to Bioequivalence Studies

2017 ◽  
Vol 8 (2) ◽  
Author(s):  
Senthil Rajan Dharmalingam ◽  
Srinivasan Ramamurthy ◽  
Sai Siddhardh ◽  
M. D. Basheerudhin
Keyword(s):  
Human Plasma ◽  
Mobile Phase ◽  
High Performance ◽  
Method Development ◽  
Diclofenac Sodium ◽  
Pharmacokinetic Studies ◽  
Chromatography Method ◽  
Method Development And Validation ◽  
Liquid Chromatography Method ◽  
Development And Validation

A new selective and sensitive high-performance liquid chromatography method was developed for the quantification of Naproxen in human plasma using diclofenac sodium asinternal standard (IS). Chromatographic separation was achieved on aPhenomenex GEMINI C18 (150 x 4.6 mm, 5 mm) column. The mobile phase consists of a mixture of Acetonitrile: 0.5% Triethylamine buffer (50:50; v/v) and the pH of the mobile phase was adjusted to 3.5 by 85 % orthophosphoric acid. Flow rate of mobile phase was 1 mL/min.Detection was performed at 230nm. The calibration curve was linear over the concentration range from 10 to 120µg/mL. The detection (LOD) and quantification (LOQ) limits were 10 ng/mL and 25 ng/Ml respectively. The method was validated for accuracy, precision, specificity, robustness, and detection and quantification limits, in accordance with ICH guidelines.The developed method for the determination of Naproxen from human plasma has been found accurate, precise, selective, and suitable for the bioequivalence and pharmacokinetic studies.

Bioanalytical Method Development of Atenolol Enantiomers: Stereoselective Behavior in Rabbit Plasma by RP-UFLC Method

2019 ◽  
Vol 16 ◽  
Author(s):  
Charan Raju C ◽  
B M Gurupadayya ◽  
Prachi Raikar
Keyword(s):  
Method Development ◽  
Pharmacokinetic Studies ◽  
Pharmacokinetic Data ◽  
Rabbit Plasma ◽  
Bioanalytical Method ◽  
Sodium Hydrogen Phosphate ◽  
Method Development And Validation ◽  
Rate Of Recovery ◽  
Fast Liquid Chromatography ◽  
Development And Validation

Objective: The objective of the method was to develop a new, simple and reliable enantioselective Reverse Phase- Ultra Fast Liquid Chromatography (RP-UFLC) method for the separation of Atenolol enantiomers. Comprehensive study was performed by extending the work to pharmacokinetic studies using rabbit plasma. Background: Many methods were reported for enantioseparation of Atenolol enantiomers but, no attempts were made for chiral separation of Atenolol using rabbit plasma. Moreover, pharmacokinetic data to prove the efficiency of particular enantiomers in rabbit plasma was not studied. Method: In the present examination, the binary RP-UFLC technique was developed on Phenomenex® Lux cellulose i5 segment (150×4.6 mm, 5µ) using di-sodium hydrogen phosphate buffer (pH 6.8): acetonitrile (35:65 v/v) as the mobile phase. Results: The elution of Atenolol was observed at 225 nm with a stream rate of 1 mL.min-1. The described technique offered a linear relationship with a regression coefficient of r2= 0.997 and 0.996 for (R) and (S)-enantiomer respectively between the concentration range of 2-10 ng.mL-1. Atenolol enantiomers were detected at a retention time (tR) of 2.7 min and 3.10 min R and S-enantiomer respectively. The rate of recovery of both Atenolol enantiomers was observed to be (R) 98.18% and (S) 100.45% individually. USFDA guidelines May 2018, were systematically followed for bioanalytical method development and validation. Conclusion: The developed technique was applied for the separation of Atenolol enantiomers and for the pharmacokinetic determination of Atenolol enantiomers in rabbit plasma.

scholarly journals BIO-ANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF AVELUMAB, AXITINIB AND ITS APPLICATION TO PHARMACOKINETIC STUDIES IN RABBIT PLASMA BY USING LCMS/MS

2021 ◽  
pp. 198-204
Author(s):  
SYED RAFI ◽  
KANTIPUDI RAMBABU
Keyword(s):  
Mobile Phase ◽  
Method Development ◽  
Internal Standard ◽  
Pharmacokinetic Studies ◽  
Rabbit Plasma ◽  
System Suitability ◽  
Method Development And Validation ◽  
Development And Validation ◽  
Stability Results ◽  
Good Agreement

Objective: An easy, quick, precise, active and reproducible LC-MS/MS technique was developed for the bioanalytical method of Avelumab and Axitinib using Cytarabine as an internal standard. Methods: This article summarizes the recent progress on bioanalytical LC-MS/MS methods using waters x-bridge phenyl column (150x4.6 mm, 3.5µ) column and organic mobile phase of 0.1% Tri fluoro acetic acid and Acetonitrile in 50:50 ratio. Results: The calibration curve was linear in the range of 2-40 ng/ml for avelumab and 0.5-10 ng/ml axitnib. Accuracy, precision, recovery, matrix effect and stability results were found to be within the suitable limits. Simple and efficient method was developed and utilized in pharmacokinetic studies to see the investigated analyte in body fluids. Conclusion: The application denotes all the parameters of system suitability, specificity, linearity and accuracy are in good agreement with USFDA guidelines and applied effectively for the investigation of pharmacokinetic studies in rabbit.

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