An RP-LC method was developed and validated for the determination of dabigatran etexilate in a capsule formulation. The LC method was carried out on a Zorbax C18 column (250 x 4.6 mm id). The mobile phase consisted of acetonitrile and a solution of triethylamine 0.1%, pH 6.0 adjusted with phosphoric acid (65 + 35, v/v) at a flow rate of 1.0 mL/min. The diode array detector was set at 225 nm. The chromatographic separation was obtained with retention time of 6.31 min, and linearity was in the range of 10-70 microg/mL (R2 = 0.9991). The specificity and stability-indicating capability of the method was proven through degradation studies and showing that there was no interference from the excipients. The accuracy was 100.23%, with an RSD of 1.34%. The LOD and LOQ were 0.04 and 10 microg/mL, respectively. Moreover, method validation demonstrated acceptable results for robustness and a system suitability test. The proposed method was applied for the analysis of the capsules to ensure their therapeutic efficacy.

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A simple, specific, rapid and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the analysis of fluticasone propionate (FP) in pharmaceutical formulations was developed and validated using deflazacort as internal standard (IS).

SummaryThe administration of 10 ml/kg b.w. of a 10−4 M ellagic acid solution to dogs primed with saline (control group) caused a marked shortening of the silicone clotting time and a mild shortening of the glass clotting time whereas no changes in the euglobulin lysis time were noted. The administration of the compound to dogs primed with Trasylol (10,000 K.I.U./kg b.w.) failed to cause any change in the clotting times but caused instead a sharp inhibition of fibrinolysis. The administration of ellagic acid to dogs primed with EACA (0.3 g/kg b.w.) caused a shortening of the silicone and glass clotting times similar to that observed in the control group whereas fibrinolysis was not significantly inhibited. These data indicate that Trasylol inhibits Hageman factor activation by ellagic acid whereas EACA has no effect.

The effects of etoricoxib on blood coagulation parameters were evaluated, along with acetylsalicylic acid, in male Wistar rats. Blood samples were collected at the end of the first, second, third and fourth weeks of the administration period and the plasma concentrations of etoricoxib determined by liquid chromatography-tandem mass spectrometry; the samples were also used for the analysis of the hematological parameters. There were no significant changes in the platelet count and fibrinogen levels, and a decrease by 1.9% of the prothrombin time was detected at the third week. The activated partial thromboplastin time assay showed a nonsignificant shortening. The antiactivated factor X and antiactivated factor II activities showed reductions lower than 2.8 and 1.3%, respectively. These findings and the comparison with acetylsalicylic acid can be helpful to support the benefit-to-risk profile, contributing to the safe therapeutic use.