HPLC method for the determination of fluvoxamine in human plasma and urine for application to pharmacokinetic studies

2007 ◽  
Vol 43 (4) ◽  
pp. 1444-1451 ◽  
Author(s):  
Sevgi Tatar Ulu
Author(s):  
Pallavi V. Duse ◽  
Kamalkishor G. Baheti

A precise, simple and reproducible reverse phase liquid chromatography (RP-HPLC) method was developed and validated for determination of Favipiravir by using Carbamazepine as internal standard in spiked human plasma. A chromatographic separation was accomplished with Cromasil C18 (250mm x 4.6ID, Particle size: 5 micron) column using mobile phase consists of methanol: water in the ratio (35:65, %v/v), at pH 3.0 with binary gradient system-maintained flow rate at 0.8ml/min. The detection wavelength of drug sample was at 225 nm. Extraction was done by using ethyl acetate as extracting solvent. The retention time of Favipiravir was found to be 6.62 min.  The method was found to be linear in the concentration range of 0.2-3.2 µg/ml. Limit of quantitation (LOQ) value was found to be 0.72. The intra- and inter day precision and accuracy lies within the specified range. The recovery studies were found to be in the range of 97.6 to 100.2%. %Relative standard deviation (RSD) was found to be in the range of 0.07-2.80%. All parameters were found to be validated from spiked human plasma. The proposed RP-HPLC method is highly accurate and rapid for the determination of favipiravir in human plasma and can be applied for pharmacokinetic studies and Therapeutic drug monitoring.


2013 ◽  
Vol 96 (5) ◽  
pp. 987-990
Author(s):  
Sevgi Tatar Ulu

Abstract A sensitive HPLC method for the determination of methoxamine in human plasma and urine is described. The method is based on derivatization of methoxamine with 4-chloro-7-nitrobenzofurazan in borate buffer of pH 9.5 to yield a yellow, fluorescent product. Isocratic HPLC separation was achieved on an Inertsil C18 column (250 × 4.6 mm id, 5 μm particle size) using the mobile phase methanol–water (60 + 40, v/v) at a flow rate of 1.2 mL/min. Fluorescence detection was used at excitation and emission wavelengths of 458 and 521 nm, respectively. The assay was linear over the concentration ranges of 10–250 and 20–300 ng/mL for plasma and urine, respectively. The LOD values were 3.3 and 6.8 ng/mL and the LOQ values were 10 and 20 ng/mL for plasma and urine, respectively. The extraction recoveries were more than 97.10%. After strict validation, the method indicated good performance in terms of linearity, sensitivity, precision, accuracy (recovery), robustness, and system suitability, and it was successfully applied to the determination of methoxamine in human plasma and urine.


2013 ◽  
Vol 2013 ◽  
pp. 1-7 ◽  
Author(s):  
Nan Wang ◽  
Liqin Zhu ◽  
Xuequn Zhao ◽  
Wenjie Yang ◽  
He Sun

Objective. To develop a simple and rapid high-performance liquid chromatography (HPLC) method for measuring moxifloxacin concentration in human plasma. Methods. Following a single step liquid-liquid extraction, analytes along with an internal standard (IS) were separated using an isocratic mobile phase of 0.1% triethylamine (adjusted pH to 4.8 with phosphoric acid)/acetonitrile (80/20, v/v) at flow rate of 1 mL/min on reverse phase Kromasil C18 column (250 mm × 4.6 mm, 5 μm) at room temperature. Results. Total analytical run time for selecting moxifloxacin was 15 min. The assays exhibited good linearity (r2=0.9998) over the studied range of 25 to 5000 ng/mL. The absolute recovery rate of low, medium, and high concentrations were 69.88%, 78.86%, and 78.51%, respectively. The relative recovery rates were 98.50%, 96.61%, and 101.79%, respectively. Coefficient of variation and error at both of the intraday and interday assessments were less than 4.7%. Conclusions. The results indicated that this method is a simple, rapid, precise and accurate assay for the determination of moxifloxacin concentrations in human plasma. This validated method is sensitive and reproducible enough to be used in pharmacokinetic studies.


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