Simultaneous Determination of Emtricitabine and Tenofovir disoproxil fumarate in Pharmaceutical Dosage by Reverse Phase High Performance Liquid Chromatography

Author(s):  
Rajan V. Rele ◽  
Sandip P. Patil

A simple, rapid and accurate high performance liquid chromatography method is described for simultaneous determination of emtricitabine and tenofovir disoproxil fumarate from active pharmaceutical ingredients. The separation of drug was achieved on Hypersil BDS C18 (150 x 4.6 mm i.d.) with 5 µ particle size column showed most favorable chromatographic pattern over the other columns. The mobile phase consisted of a mixture of buffer and methanol (85:15 % v/v). The buffer was mixtures of 0.1 % (v/v) ortho-phosphoric acid solution adjusted the pH 3.5 with tri-ethyl amine. The detection was carried out at wavelength 260 nm. The mixture of buffer of pH 3.5 and methanol (85:15% v/v) was used as a diluent. The method was validated for system suitability, linearity, accuracy, precision, robustness, stability of sample solution. The method has been successfully used to analyze emtricitabine and tenofovir disoproxil fumarate from active pharmaceutical ingredients.

2020 ◽  
Vol 103 (4) ◽  
pp. 1181-1189
Author(s):  
Xiaoyun Duan ◽  
Xiaofeng Liu ◽  
Yue Dong ◽  
Jing Yang ◽  
Jing Zhang ◽  
...  

Abstract Background Sulfonamides have been widely used in the prevention and clinical treatment of bacterial diseases in livestock and poultry. The use of sulfonamides increases the risk of veterinary drug residues in animal derived foods. The traditional reversed phase liquid chromatography methods for sulfonamides residues detection in animal derived foods have the problem of high consumption of organic solvents. Objective The aim of this study was to establish a green high-performance liquid chromatography method for the detection of sulfonamides residues in different animal-origin foods. Method The sample extraction solutions were purified by the Agela Cleanert PEP-2 cartridge and analyzed by the high-performance liquid chromatography method using ethanol as the green alternative solvent. Results The proposed method was validated in terms of linear range (20–1000 μg/kg), limit of detection (3.0–12.3 μg/kg), limit of quantitation (10–43 μg/kg), accuracy (80.7–101.3%), and repeatability and reproducibility (RSD <5.9% and RSD <8.5% respectively). Conclusions The proposed method is an environmentally friendly, sensitive and reliable high-performance liquid chromatography method for simultaneous determination of sulfonamide residues in animal-origin foods. Highlights In this work, we firstly developed a green high-performance liquid chromatography method for simultaneous determination of the residues of nine sulfonamides in milk and beef with ethanol as the green alternative solvent.


2012 ◽  
Vol 57 (1) ◽  
pp. 484-489 ◽  
Author(s):  
Mei Zhang ◽  
Grant A. Moore ◽  
Murray L. Barclay ◽  
Evan J. Begg

ABSTRACTA rapid and simple high-performance liquid chromatography (HPLC) assay was developed for the simultaneous determination of three triazole antifungals (voriconazole, posaconazole, and itraconazole and the metabolite of itraconazole, hydroxyitraconazole) in human plasma. Sample preparation involved a simple one-step protein precipitation with 1.0 M perchloric acid and methanol. After centrifugation, the supernatant was injected directly into the HPLC system. Voriconazole, posaconazole, itraconazole, its metabolite hydroxyitraconazole, and the internal standard naproxen were resolved on a C6-phenyl column using gradient elution of 0.01 M phosphate buffer, pH 3.5, and acetonitrile and detected with UV detection at 262 nm. Standard curves were linear over the concentration range of 0.05 to 10 mg/liter (r2> 0.99). Bias was <8.0% from 0.05 to 10 mg/liter, intra- and interday coefficients of variation (imprecision) were <10%, and the limit of quantification was 0.05 mg/liter.


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