The Analytical method (HPLC) used for identification, assay of triclabendazole, related substances and preservatives used in finished product Tricladem 5, in SC Delos Impex 96 SRL

Authors: Maria Neagu, Cristina I. Marinescu, Roxana M. Covaci, Catalina S. Macovei                           Affiliation: SC Delos Impex ’96 SRL, Bucharest, RO.

Because, triclabendazole is an active pharmaceutical ingredient without compendial monography (European Pharmacopoeia, United Stated Pharmacopoeia)  in SC Delos Impex ’96 SRL, the API identification, assay, related substances, and, preservatives, assay and identification  is efectuated used the method presented below.  Presented original method permit, all these determination in a relative short time  (the chromatogram time recorded  is 25 min.).

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Some aspects regarding impurities profile in fipronil – HPLC method

Authors: Ana Csuma, Cornelia Pîrlog                                                                                             Affiliation: S.N. Institutul Pasteur S.A., Bucuresti

Using a substance as active pharmaceutical ingredient in veterinary drug formulation requires the characterization of this substance as content in active compound and so in terms of impurities possible present in it, the latter being a mandatory requirement for a drug application. Fipronil is a synthetic product belonging to pesticide class used in veterinary practice to manufacture of some products against fleas, given spot–on or in form of spray, in cats and dogs. The main impurities in fipronil include process related impurities and degradation products as a result of exposure to environmental conditions: reduction, oxidation, photolysis and hydrolysis. A HPLC method suitable for analytical separation of fipronil from its impurities was established. Separation was achieved on a reversed phase column using a mixture of methanol, acetonitrile and water as mobile phase. In the chosen chromatographic conditions the resolution between fipronil and its sulphone (the main impurity) was >3 and the tailing factor (T) < 2.0. Related impurities have absorbed in the same band of UV wavelength as the main compound fipronil. Comparing the area of impurities obtained for sample solution with the area of the main peak in diluted standard solution allowed the detection of impurities at concentration

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The validation of the Analytical method (HPLC), use for identification and assay of the pharmaceutical active ingredient, colistine sulphate and the finished product Colidem 50 – hydrosoluble powder, in SC DELOS impex ‘96 SRL

Authors: Maria Neagu, Cristina Marinescu, Carmen Popescu                                                         Affiliation: SC DELOS IMPEX ’96 SRL, Bucuresti

In SC DELOS IMPEX ’96 SRL the quality of the active pharmaceutical ingredient (API) for the finished product Colidem 50 – hydrosoluble powder is make according to European Pharmacopoeia, curent edition. The method for analysis use in this purpose is the compendial method „Colistine sulphate” in E.P. in current edition and represent a optimized variant, developed and validated „in house”.The parameters which was included in the methodology validation for chromatographic method are the follow: selectivity/specificity, linearity, range of linearity, limit of detection and limit of quantification, precision (repeatability-intra day, inter-day reproducibility), accuracy, robustness, stability solutions and system suitability.

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