Quantification of active pharmaceutical ingredients in commercially available poly pharmaceutical tablets by means of DSC

Differential scanning calorimetry is the first line technique indispensable for industrial quality controllaboratories and, next to many routine applications, could be used in quantitative assays. For this purpose, a relationship between the signal value of analyte (enthalpy change ΔH) and its concentration in the matrix isused. However, there are several limitations of its application, concerning solid state interactions between APIs, other APIs and/or coexisting excipients. With respect to their physical properties, it is known that amorphization state and/or permanent particle deformation can produce relatively large areas of interparticle contact and thus high particle-particle bonding forces. Finally, it may affect the DSC quantitative measurements. The problem was shown using commercially available, different poly component tablets containing ibuprofen in the presence of pseudoephedrine hydrochloride or paracetamol and coexisting excipients

The influence of ionizing radiation on itraconazole in the solid state

The aim of this study was to investigate the ionizing radiation effects, in the form of an electron beam, on itraconazole (ITR) in the solid phase. It was found that the ITR, under the influence of a standard 25 kGy dose of radiation used for the sterilization of drug substances, decomposed at 0.4%. Moreover, a gentle change of colour and a decrease in melting point does not exceed pharmacopoeial standards causing that ITR can be sterilized by radiation method. The use of high 400 kGy radiation doses resulted in a 6.5% decomposition of the ITR and eight radiodegradation products were found. However, with the exception of differential scanning calorimetry (DSC), the X-ray diffraction, Fourier transform infrared spectroscopy (FT-IR) and ultraviolet-visible (UV-vis) methods showed no changes in the form and the morphology of the crystals. The structures of all those compounds were investigated. It was confirmed that the ITR decomposition takes place by dehalogenation (one of Cl atom elimination), the oxidation in isobutyl residue (beside the triazole ring) and C-O bond rupture

Photodegradation assessment of amisulpride, doxepin, haloperidol, risperidone, venlafaxine, and zopiclone in bulk drug and in the presence of excipients

Photostability of amisulpride, doxepin, haloperidol, risperidone, venlafaxine, and zopiclone in APIs and powdered tablets during exposure to UVA irradiation was studied. In order to evaluate the photodegradation process an ultrahigh performance liquid chromatography method coupled with tandem mass spectrometry (UHPLC-MS/MS) was developed and validated. It was found that the photodegradation of the studied compounds depends on the type of drug and co-existing excipients. Different percentage of photodegradation of the studied drugs was observed, and therefore amisulpride decomposed at 2.63% in bulk drug and at 5.74% in pharmaceutical preparation, doxepin: 29% and 72.38%, haloperidol: 3.71% and 26.20%, risperidone: 7.13% and 12.86%, venlafaxine: 38.59% and 4.22%, zopiclone: 18.62% and 31.42% respectively, after 114 days of UVA irradiation. In addition, kinetic evaluation of the photodegradation process was performed by determining the order of reaction, reaction rate constant k and time $t_{0.1}$ and $t_{0.5}$. The photodegradation products of studied drugs were identified, and their fragmentation pathways, derived from MS/MS data, were proposed. The photostability testing is an integral part of the drug stability assessment to ensure quality, efficacy and safety of the formulated products during manufacturing process, storage as well as normal use

Photodegradation assessment of ciprofloxacin, moxifloxacin, norfloxacin and ofloxacin in the presence of excipients from tablets by UPLC-MS/MS and DSC

Background: Ciprofloxacin (CIP), moxifloxacin (MOX), norfloxacin (NOR) and ofloxacin (OFL), are the antibacterial synthetic drugs, belonging to the fluoroquinolones group. Fluoroquinolones are compounds susceptible to photodegradation process, which may lead to reduction of their antibacterial activity and to induce phototoxicity as a side effect. This paper describes a simple, sensitive UPLC-MS/MS method for the determination of CIP, MOX, NOR and OFL in the presence of photodegradation products. Results: Chromatographic separations were carried out using the Acquity UPLC BEH C18 column; (2.1 × 100 mm, 1.7 μm particle size). The column was maintained at 40°C, and the following gradient was used: 0 min, 95% of eluent A and 5% of eluent B; 10 min, 0% of eluent A and 100% of eluent B, at a flow rate of 0.3 mL min-1. Eluent A: 0.1% (v/v) formic acid in water; eluent B: 0.1% (v/v) formic acid in acetonitrile. The method was validated and all the validation parameters were in the ranges acceptable by the guidelines for analytical method validation. The photodegradation of examined fluoroquinolones in solid phase in the presence of excipients followed kinetic of the first order reaction and depended upon the type of analyzed drugs and coexisting substances. Photodegradation process of analyzed drugs was confirmed by differential scanning calorimetry. In addition, the identification of degradation products was carried out by mass spectrometry. Conclusion: The developed UPLC-MS/MS method enables the determination of CIP, MOX, NOR and OFL in the presence of photodegradation products and identification of photodegradation products

Semiautomatic and fully functional electrochemical microanalyzer BO-05 suitable for scientific, didactic, and analytical applications : the use in the potentiometric analysis of drugs

This article presents the potentiometric method of determination of chlorides using the original BO-05 electrochemical microanalyzer. The quantification of chlorides is one of the frequently performed methods, both in the indirect determination of active pharmaceutical ingredients (API) and impurities in pharmaceutical raw materials, pharmacopoeial substances or pharmaceutical formulations as well. Successfully validated method was used to the analysis of chlorides in the preparations containing verapamil hydrochloride in form of tablets Staveran® and Verapamil® . The mean content of the studied API calculated to one tablet was close to the declared and equal to 123.6±1.5 mg and 122.6±1.1 mg, respectively. The presence of excipients have no significant impact on the final results. Thus shown that the electrochemical microanalyzer BO-05 is suitable for scientific, didactic and analytical applications

Semiautomatic and fully functional electrochemical microanalyzer BO-05 suitable for scientific, didactic, and analytical applications: The use in the potentiometric analysis of drugs

This article presents the potentiometric method of determination of chlorides using the original BO-05 electrochemical microanalyzer. The quantification of chlorides is one of the frequently performed methods, both in the indirect determination of active pharmaceutical ingredients (API) and impurities in pharmaceutical raw materials, pharmacopoeial substances or pharmaceutical formulations as well. Successfully validated method was used to the analysis of chlorides in the preparations containing verapamil hydrochloride in form of tablets Staveran® and Verapamil®. The mean content of the studied API calculated to one tablet was close to the declared and equal to 123.6±1.5 mg and 122.6±1.1 mg, respectively. The presence of excipients have no significant impact on the final results. Thus shown that the electrochemical microanalyzer BO-05 is suitable for scientific, didactic and analytical applications