Development and validation of ultra-performance liquid chromatography method for the determination of meloxicam and its impurities in active pharmaceutical ingredients

2018 ◽  
Vol 76 (3) ◽  
pp. 187-200 ◽  
Author(s):  
K. Louati ◽  
I. Bargaoui ◽  
F. Safta
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.


2014 ◽  
Vol 58 (4) ◽  
pp. 621-629 ◽  
Author(s):  
Wojciech Jerzy Pietro ◽  
Aneta Woźniak ◽  
Katarzyna Pasik ◽  
Wojciech Cybulski ◽  
Dorota Krasucka

Abstract A liquid chromatography-ultraviolet detection method for the determination of florfenicol (FF) and thiamphenicol (TAP) in feeds is presented. The method comprises the extraction of analytes from the matrix with a mixture of methanol and acetonitrile, drying of the extract, and its dissolution in phosphate buffer. The analysis was performed with a gradient programme of the mobile phase composed of acetonitrile and buffer (pH = 7.3) on a Zorbax Eclipse Plus C18 (150 × 4.6 mm, 5 μm) analytical column with UV (λ = 220 nm) detection. The analytical procedure has been successfully adopted and validated for quantitative determination of florfenicol and thiamphenicol in feed samples. Sensitivity, specificity, linearity, repeatability, and intralaboratory reproducibility were included in the validation. The mean recovery of amphenicols was 93.5% within the working range of 50-4000 mg/kg. Simultaneous determination of chloramphenicol, which is banned in the feed, was also included within the same procedure of FF and TAP stability studies. Storing the medicated feed at room temperature for up to one month decreased concentration in the investigated drugs even by 45%. These findings are relevant to successful provision of therapy to animals.


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