scholarly journals Development and Validation of a Stability- Indicating High Pressure Liquid Chromatography Method for Determination of Prostaglandin E1 and its Degradation Products in sn Intracavernous Formulation

2013 ◽  
Vol 04 (04) ◽  
Author(s):  
Victoire Vieillard
Author(s):  
Adriane Lettnin Roll Feijó ◽  
Fernanda Macke Hellwig ◽  
Clésio Soldateli Paim ◽  
Marcelo Donadel Malesuik

This study aimed to develop and validate a stability-indicating liquid chromatography method for the determination of tirofiban hydrochloride and two synthetic impurities (impurity A and impurity C). The method utilizes a RP-18 column (250 mm × 4.6 mm; 5 μm) with the PDA detector for quantitation. A mixture of triethylamine 0.1% (acidified to pH 5.5 with phosphoric acid) and acetonitrile was used as the mobile phase at a flow rate of 1 mL min−1 with gradient elution. The method presented satisfactory linearity, precision, accuracy and robustness, as well as low limits of detection and quantification, which demonstrate sensitivity in the determination of tirofiban and impurities A and C. It was selective for the determination of the drug and impurities analysed, without interference of the degradation products generated under forced conditions, demonstrating the stability-indicating capacity of the proposed method. Tirofiban showed to be practically stable to oxidative (30% H2O2 for 24 h) and thermal (75 ºC for 24 h) conditions, but presented degradation to UVA light and acid hydrolysis, obeying the first order kinetics for both. In this way, it can be used as a stability-indicating method in the quality control of the raw material of tirofiban hydrochloride, as well as of the finished product. The obtained results demonstrate the importance of deepening the studies in this area, in order to guarantee the quality of commercialized pharmaceutical products.


2006 ◽  
Vol 69 (11) ◽  
pp. 2712-2719 ◽  
Author(s):  
VINCENZO LIPPOLIS ◽  
MICHELANGELO PASCALE ◽  
ANGELO VISCONTI

A fluorescence polarization immunoassay previously described for deoxynivalenol (DON) screening in wheat was optimized for the rapid quantification of DON in durum wheat kernels, semolina, and pasta. A background signal was observed in both spiked and naturally contaminated samples, strictly depending on the testing matrix. After subtracting the background DON level for durum wheat (0.27 μg of DON per g), semolina (0.08 μg of DON per g), and pasta (0.04 μg of DON per g), an accurate quantification of DON was possible at levels greater than 0.10 μg/g for all matrices. Average recoveries from spiked samples (0.25 to 1.75 μg/g) were 98, 102, and 101% for wheat, semolina, and pasta, respectively. Comparative analyses of 35 naturally contaminated durum wheat samples, 22 semolina samples, and 26 pasta samples performed by both the fluorescence polarization method and high-pressure liquid chromatography/immunoaffinity cleanup showed a good correlation (r > 0.995). The fluorescence polarization method showed better accuracy and precision with respect to the high-pressure liquid chromatography method and is suitable for the rapid and quantitative determination of DON in durum wheat–based products at levels foreseen by existing or coming international regulations.


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