Now showing 1 - 10 of 18
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    Development and optimization of a generic HPLC method for the simultaneous determination of common ingredients in multi component cough and cold oral drug products using chemometrics
    (Macedonian Pharmaceutical Association, 2018)
    Zafirova, Marija
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    Ugrinova, Liljana
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    Petrovska-Dimitrievska, Gabriela
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    Karchev, Vasil
    <jats:p>The aim of this work was to develop a single, generally applicable high performance liquid chromatography/diode array detector (HPLC/DAD) method for simultaneous determination of the most frequently used cough and cold active substances and their impurities that would be applicable for a number of possible formulation compositions of cough and cold medicines. The compounds that are separated by the method include eleven active substances: paracetamol, phenylephrine HCl, caffeine, ibuprofen, ascorbic acid, propiphenazone, pheniramine maleate, chlorphenamine maleate, pseudoephedrine HCl, dextromethorphan HBr and cetylpyridinium Cl; five of their impurities: 4-aminophenol, 4-nitrophenol, 4`-chloroacetanilide, chlorphenamine impurity C and ephedrine HCl; and two preservatives: sodium benzoate and propyl parahydroxybenzoate. All 18 compounds were successfully separated on a reversed phase (RP)-HPLC column with superficially porous particles using gradient elution with a very simple mobile phase in 14 minutes with excellent sensitivity and resolution. Method optimization was performed by the design of experiments approach. The proposed method has been validated according to ICH guidelines and proved to be suitable for the simultaneous qualitative and quantitative determination of the selected compounds in different cough and cold dosage forms. Keywords: cough and cold active substances and impurities, HPLC/DAD, superficially porous particles, core-shell particles, chemometrics, design of experiments</jats:p>
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    Development of a stability-indicating method for evaluation of impurity profile of Atorvastatin film-coated tablets using cyano column based on core-shell technology
    (Society of Chemists and Technologists of Macedonia, 2022-06-30)
    Trajchova Kovachovska, Elena
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    Trajkovic, Stefan
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    Mitrevska, Ivana
    <jats:p>This research highlights the specificity of the new stability-indicating method developed to evaluate the impurity profile of Atorvastatin film-coated tablets. The proposed method has the ability to capture any possible changes that may occur during the stability studies over time and under different stress factors, and is selective enough to enable quality control of finished product from different suppliers of active pharmaceutical ingredient (API)/excipients.  Satisfactory critical peak resolution between specified and unspecified impurities was achieved using the fused-core shell technology and extensively endcapped diisopropyl-cyanopropylsilane stationary phase (Halo ES-CN 150 mm × 4.6 mm, 2.7 µm), with a 10 mM ammonium formate buffer pH 3.5 and acetonitrile as mobile phase. A potential worse case impurity profile was assumed by using retained samples combined with the data obtained for samples manufactured with APIs from different suppliers exposed to the forced degradation study. The mass balance for stressed samples demonstrated the stability-indicating capability of the proposed method.</jats:p>
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    Possibilities and challenges of "green" chromatographic solutions
    (Macedonian Pharmaceutical Association, 2022-12-31)
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    Chromatographic and Surfactant Based Potentiometric Determination of Aqueous Dissociation Constant of Mupirocin
    (Bentham Science Publishers Ltd., 2020-02-11)
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    Karchev, Vasil
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    <jats:sec> <jats:title>Background:</jats:title> <jats:p>The available data concerning aqueous dissociation constant of mupirocin (sparingly soluble drug) are scarce. In this study, chromatographic, surfactant based potentiometric concept and spectrophotometric method were used for determination of the aqueous pKa value of mupirocin.</jats:p> </jats:sec> <jats:sec> <jats:title>Methods:</jats:title> <jats:p>Different approaches were used for estimation of the aqueous pKa value from the apparent pKa values obtained at four ACN concentrations, ranging from 22% to 30%. The potentiometric determination of the pKa value of mupirocin was performed using different concentration of Tween 80 as a surfactant.</jats:p> </jats:sec> <jats:sec> <jats:title>Results:</jats:title> <jats:p>The aqueous pKa value of mupirocin, determined for the first time by reverse-phase liquid chromatography method, was found to be 4.76. The obtained value was confirmed by potentiometric method (4.85). It was found that Tween 80 increases the pKa values. The linear relationship between the apparent pKa values and the surfactant concentrations was used as an approach for estimation of the aqueous pKa value. Both methods gave similar values for aqueous pKa which correspond with the theoretically obtained pKa value (4.88) using Pallas computer program. It was found that mupirocin gives pH-indipendent spectra, thus spectrophotometric method is not applicable for determination of pKa of this compound.</jats:p> </jats:sec> <jats:sec> <jats:title>Conclusion:</jats:title> <jats:p>This comprehensive approach used for the pKa determination enable us to obtained reliable results for the aqueous pKa value of mupirocin. The linear relationship between the pKa values and the nonionic surfactant concentrations could be used as a reliable and simple approach for determination of aqueous pKa value of sparingly soluble drugs.</jats:p> </jats:sec>
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    Scientific approach and implementation of a measurement uncertainty in mass balance determination
    (Macedonian Pharmaceutical Association, 2022-12-31)
    Hadzieva Gigovska, Maja
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    Optimization of ion-suppression reverse phase-separation of basic compounds using different mobile phases
    (Macedonian Pharmaceutical Association, 2022-12-31)
    Petrovska Dimitrievska, Gabriela
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    Zafirova Gjorgievska, Marija
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    Ugrinova, Liljana
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    Implementation of quality by design principles in the development of microsponges as drug delivery carriers: Identification and optimization of critical factors using multivariate statistical analyses and design of experiments studies
    (Elsevier BV, 2015-07-15)
    Simonoska Crcarevska, Maja
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    Slavevska Raicki, Renata
    Microsponges drug delivery system (MDDC) was prepared by double emulsion-solvent-diffusion technique using rotor-stator homogenization. Quality by design (QbD) concept was implemented for the development of MDDC with potential to be incorporated into semisolid dosage form (gel). Quality target product profile (QTPP) and critical quality attributes (CQA) were defined and identified, accordingly. Critical material attributes (CMA) and Critical process parameters (CPP) were identified using quality risk management (QRM) tool, failure mode, effects and criticality analysis (FMECA). CMA and CPP were identified based on results obtained from principal component analysis (PCA-X&Y) and partial least squares (PLS) statistical analysis along with literature data, product and process knowledge and understanding. FMECA identified amount of ethylcellulose, chitosan, acetone, dichloromethane, span 80, tween 80 and water ratio in primary/multiple emulsions as CMA and rotation speed and stirrer type used for organic solvent removal as CPP. The relationship between identified CPP and particle size as CQA was described in the design space using design of experiments - one-factor response surface method. Obtained results from statistically designed experiments enabled establishment of mathematical models and equations that were used for detailed characterization of influence of identified CPP upon MDDC particle size and particle size distribution and their subsequent optimization.
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    Design of experiments (DoE) to model phenolic compounds recovery from grape pomace using ultrasounds
    (Springer Science and Business Media LLC, 2021-11-22)
    Ćućuz, Veljko
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    Cvejić, Jelena
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    Torović, Ljilja
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    Gojković-Bukarica, Ljiljana
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