66 research outputs found

    Grouping of residual solvents present in pharmaceuticals using experimental planning and chemometric methods

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    The main effects of six experimental factors on the efficiency of HS (headspace) extraction in headspace gas chromatography – flame ionization detector (HS-GC-FID) determination of twenty organic solvents routinely used in production of pharmaceuticals were obtained on the basis of the results of experiments carried out according to the Plackett-Burman factorial design. The effects were used as a basis for grouping the solvents into five groups, the solvents belonging to a group responded similarly to changes of HS conditions. To this end, visualization approaches were used as well as chemometric methods: cluster analysis (CA) and principal component analysis (PCA). Moreover, the most important HS experimental factors were selected for further optimization of the HS-GC determination procedure

    Simplex optimization of headspace factors for headspace gas chromatography determination of residual solvents in pharmaceutical products

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    The purpose of the present work was to find optimum conditions of headspace gas chromatography (HS-GC) determination of residual solvents which usually appear in pharmaceutical products. Two groups of solvents were taken into account in the present examination. Group I consisted of isopropanol, n-propanol, isobutanol, n-butanol and 1,4-dioxane and group II included cyclohexane, n-hexane and n-heptane. The members of the groups were selected in previous investigations in which experimental design and chemometric methods were applied. Four factors were taken into consideration in optimization which describe HS conditions: sample volume, equilibration time, equilibrium temperature and NaCl concentration in a sample. The relative GC peak area served as an optimization criterion which was considered separately for each analyte. Sequential variable size simplex optimization strategy was used and the progress of optimization was traced and visualized in various ways simultaneously. The optimum HS conditions appeared different for the groups of solvents tested, which proves that influence of experimental conditions (factors) depends on analyte properties. The optimization resulted in significant signal increase (from seven to fifteen times)

    Separation and purification of curcumin using novel aqueous two-phase micellar systems composed of amphiphilic copolymer and cholinium ionic liquids

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    Novel aqueous two-phase micellar systems (ATPMS) composed of Pluronic F68, a triblock amphiphilic copolymer, and cholinium-based ionic liquids (ILs) were formulated and applied for separation/purification of curcumin (CCM). CCM stability in the presence of ATPMS components was also evaluated. CCM is stable up to 24 h in copolymer (1.0 10.0 wt%) and ILs (0.1 3.0 M) aqueous solutions. Very mild phase separation conditions (close to room temperature) were achieved by adding cholinium ILs to the Pluronic F68 + McIlvaine buffer at pH 6.0 solution. The decrease of cloud-point temperature is dependent on the relative hydrophobicity of IL anion, [Hex] > [But] > [Prop] > [Ac] > Cl. ATPMS composed of more hydrophobic ILs ([Ch][Hex] > [Ch][But] > [Ch][Prop]) are most efficient in the partition of commercial CCM into polymeric micelles-rich phase. The best ATPMS (0.70 M [Ch][But] and 0.60 M [Ch][Hex]-based ATPMS) were then used to purify CCM from a crude extract of Curcuma longa L. Both systems were very selective to separate CCM from protein-based contaminants (selectivity values 25; purification yields 12-fold). Pluronic F68-based ATPMS are promising for selective separation of hydrophobic biomolecules by using cholinium-based ILs as adjuvants to adjust phase separation temperatures and biomolecules partition.This study was funded by the Coordination for Higher Level Graduate Improvements (CAPES/Brazil, finance code 001), National Council for Scientific and Technological Development (CNPq/Brazil) and the State of São Paulo Research Foundation (FAPESP/Brazil, processes #2014/16424-7, #2017/10789-1, #2018/10799-0, #2018/05111-9; #2019/05624-9, and #2019/08549-8). A.M. Lopes and J.F.B. Pereira are grateful for the language revision of native speaker H.S. Pacheco Neto.info:eu-repo/semantics/publishedVersio

    3D inkjet printing of tablets exploiting bespoke complex geometries for controlled and tuneable drug release

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    A hot melt 3D inkjet printing method with the potential to manufacture formulations in complex and adaptable geometries for the controlled loading and release of medicines is presented. This first use of a precisely controlled solvent free inkjet printing to produce drug loaded solid dosage forms is demonstrated using a naturally derived FDA approved material (beeswax) as the drug carrier and fenofibrate as the drug. Tablets with bespoke geometries (honeycomb architecture) were fabricated. The honeycomb architecture was modified by control of the honeycomb cell size, and hence surface area to enable control of drug release profiles without the need to alter the formulation. Analysis of the formed tablets showed the drug to be evenly distributed within the beeswax at the bulk scale with evidence of some localization at the micron scale. An analytical model utilizing a Fickian description of diffusion was developed to allow the prediction of drug release. A comparison of experimental and predicted drug release data revealed that in addition to surface area, other factors such as the cell diameter in the case of the honeycomb geometry and material wettability must be considered in practical dosage form design. This information when combined with the range of achievable geometries could allow the bespoke production of optimized personalised medicines for a variety of delivery vehicles in addition to tablets, such as medical devices for example

    New wonderful world after a disaster. "Pożegnanie jesieni" by Stanisław Ignacy Witkiewicz as antyutopia.

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    Zadaniem niniejszej pracy jest spojrzenie na powieść "Pożegnanie jesieni" jak na antyutopię.The purpose of this study is to look at the novel "Pożegnanie jesieni" as dystopia

    Die Sammlung von Tschernowitz 1781-1945 (1975)

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    Die gegenwärtig im Archidiözesanmuseurn in Lemberg (Lviv) aufbewahrte „Sammlung von Tschernowitz" entstand im Ergebnis der Suche nach kirchlichen Dokumenten in der Ukraine und ihrer Rettung. Die im Jahre2002 von Tschernowitz. nach Lemberg gebrachten Akten stammen aus der Zeit von 1781 bis 1945 (mit einigen Dokumenten aus späteren Jahren) und entstanden in verschiedenen Kanzleien, was bei ihrer Einteilung in Gruppen berücksichtigt wurde. Es gibt 8 Gruppen: I - Generalvikariat (Apostolische Administratur der Bukowina) 1921-1945, II - Dekanate (1781) 1786-1929, 111 - Militärseelsorge 1804-1915, IV -Pfarreien 1786-1945 (1975), V - Schulwesen, Institutionen und Organisationen zur Wohlfahrtspflege, Vereine und Orden 1890-1942, VI - Verschiedenes (u.a. Flugschriften, Dokumentenmuster, Skripte), VII - Fremddokumente 1859-1953, VIII - die Hinterlassenschaft von P. Franciszek Krajewski ( diese Gruppe wird zur Zeit noch geordnet). Trotz unterschiedlicher Quellen der Aktenentstehung wurde beschlossen, sie in einer gemeinsamen Sammlung aufzubewahren, weil sie so gefunden worden waren und weil ihr Miteinander die Spezifik der katholischen Kirche in der Bukowina besser widerspiegelt. Die über 8 laufende Meter zählende Sammlung ist - trotz beträchtlicher Lücken, besonders in den Pfarrbüchern - in physischer Hinsicht in gutem Zustand erhalten und kann neue Materialien für historische Untersuchungen liefern

    Teaching Sensitivity - Contemporary Polish Poetry in a Polish Class in Middle School

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    Zadaniem niniejszej pracy jest podjęcie namysłu nad nauczaniem współczesnej polskiej poezji w szkole, nad problemami interpretacyjnymi oraz próba rozwiązania zdiagnozowanych problemów.Objective of this work is to take the reflection on the teaching of contemporary Polish poetry in school, on the interpretation problems and attempt to solve the problems diagnosed
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