scholarly journals Bioanalytical Method Development and Validation of Ferrum in Rabbit Plasma Samples by Derivatised Reverse Phase Liquid Chromatography and Application to Pharmacokinetic Study

Author(s):  
Geervani P ◽  
Kavitha S ◽  
Suresh PV ◽  
Prabahar AE ◽  
Rama Rao N
2019 ◽  
Vol 16 ◽  
Author(s):  
Charan Raju C ◽  
B M Gurupadayya ◽  
Prachi Raikar

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.


2020 ◽  
Vol 16 ◽  
Author(s):  
Kishor Kumar Erukulla ◽  
Suseem S.R

Objective: A particular, easy and precise reverse phase liquid chromatographic technique was developed for the determination of Zaltoprofen in human plasma. Methods: The ODS C18 (250mm x 4.6mm, 5µm) column was utilized for determination. The mobile phase contains buffer and acetonitrile (55:45 v/v). The rate of flow was 1.0 ml/min. The volume of sample infused was 10 µl. The column has been kept at a temperature of ~300C. The column was equilibrated for no less than 30 min prior to injection of the solutions. The detection wavelength was set at of 331 nm. Results: The linearity experiment was performed for Zaltoprofen in the range of 0.15 to 20 µg/ml. The observed recovery of Zaltoprofen was 98.32 %. Conclusion: The suggested technique has been validated and the same is very helpful for zaltoprofen determination in human plasma.


Author(s):  
S. SATHESHKUMAR ◽  
V. MURUGANANTHAM

Objective: The current research work focus to simple and rugged bioanalytical method development and validation of brivudine in human plasma using high-performance liquid chromatography. Methods: The analyte (Brivudine) and internal standard (Sofosbuvir) were extracted using the Solid Phase Extraction (SPE) technique. The chromatographic separation was accomplished by using Zorbax eclipse XDB-C18 Column (150×4.6 mm, 5 μm) with a mobile phase consisted of Methanol: 0.5% Ortho-phosphoric acid (65:35%, v/v) respectively, at a flow rate of 0.7 mL/min. The developed method was validated by performing system suitability, carryover effect, linearity, selectivity, sensitivity, precision, accuracy, recovery, ruggedness, and stability studies. The method was validated as per USFDA guidelines. Results: The selected chromatographic condition was found to efficiently separated brivudine (RT-3.55 min) and ISTD (RT-7.87 min). The assay demonstrated a linear dynamic range of 85.205 to 4500.246 ng/ml for brivudine in human plasma with r2>0.99. Demonstrated the lowest limit of detection at 85.205 ng/ml. This method established an intra-run and inter-run precision within the range of 2.99-6.31%CV and 3.67-5.80%CV, respectively. Additional intra-run and inter-run accuracy were within the range of 97.55-105.37% and 99.27-102.15%, respectively. The mean percentage recovery of brivudine and ISTD studies proved good extraction efficiency and the robustness was also evaluated. Conclusion: A simple, accurate, precise, linear and rugged RP-HPLC method was developed and validated for the estimation of brivudine in human plasma with K2EDTA anticoagulant and suitable for conducting BA/BE and TDM.


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