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Batch Method (batch + method)
Selected AbstractsEarly stages of protein crystallization as revealed by emerging optical waveguide technologyJOURNAL OF APPLIED CRYSTALLOGRAPHY, Issue 3 2008Attia Boudjemline A highly sensitive method for studying the onset of protein crystallization in real time using an optical-waveguide-based technique is reported. Dual polarization interferometry uses light from sensing and reference waveguides to produce an interference pattern, which when the sensing waveguide is immersed in a protein solution supplies information on the thickness and density of any protein adlayer on the sensing waveguide's surface. This technique provides evidence that crystallization proceeds via large protein aggregates but, more strikingly, shows dramatic light loss from the sensing waveguide at a very early stage during crystallization. The technique proves relatively insensitive to the crystallization of small molecules or poorly formed protein crystals and affords a method of distinguishing crystal formation from the formation of other protein aggregates or salt crystals. The experimental setup currently necessitates crystallization using the batch method, and precipitant mixing at high supersaturation is known to introduce a greater variability compared with methods such as vapour diffusion or dialysis, but first results promise to bridge the paucity of real-time methods available to distinguish the onset of protein crystallization from other forms of aggregation. [source] Wet granulation as innovative and fast method to prepare controlled release granules based on an ion-exchange resinJOURNAL OF PHARMACEUTICAL SCIENCES, Issue 3 2008Beatrice Albertini Abstract The goal of this work was to evaluate the suitability of wet granulation as an innovative and fast method for the preparation of granules containing a drug,resin complex (resinate), having cholestyramine as resin and potassium diclofenac (KD) as drug. Resinate and granules were prepared directly by steam granulation in high shear mixer (method A), using two different amount of resin (granules 1 and 2). For comparison granules 1 were also prepared by conventional batch method followed by steam granulation (method B). All granules showed quite irregular shape, main size fractions between 75 and 500 µm, good flowability and uniform KD distribution. Granules 1A exhibited controlled release profiles at pH 7.4, while granules 2A showed a burst effect due to KD free crystals. FT-IR studies confirmed the complete complexation between resin and KD during the granulation process with method A for granules 1. Finally, the dissolution test of granules 1A in different media revealed a controlled drug release in 12 h, providing the utility of this system for enteric drug delivery. Granules 1B evidenced similar characteristics to those of granules 1A; the drawback of the multistep procedure was related to the long processing time. © 2007 Wiley-Liss, Inc. and the American Pharmacists Association J Pharm Sci 97:1313,1324, 2008 [source] Selective enrichment of trace copper(II) from biological and natural water samples by SPE using ion-imprinted polymerJOURNAL OF SEPARATION SCIENCE, JSS, Issue 6-7 2008Yunhui Zhai Abstract A novel Cu(II)-imprinted polymer sorbent was prepared by an ion-imprinted polymer (IIP) technique using (2Z)- N,N,-bis(2-aminoethylic)but-2-enediamide as the functional monomer and pentaerythritol triacylate as a crosslinker. IR, XPS, and elemental analysis techniques were used to confirm the obtained product. Subsequently, when this polymer was used as sorbent in SPE, it exhibited excellent selectivity for template ion from an aqueous solution. Quantitative extraction of Cu(II) was achieved in the pH range of 4,7. The time needed to extract each sample was less than 30 min by the batch method. The distribution ratio (D) values of IIP for Cu(II) were greatly larger than that for other ions. At optimal pH value, the maximum extraction capacity of IIP and nonimprinted polymer (NIP) was found to be 29.8 and 7.0 mg/g, respectively. The adsorption behavior of Cu(II) on the sorbents could be described by Langmuir adsorption isotherm equation. The feasible flow rate of Cu(II)-containing solution for quantitative extraction onto the column packed with IIP was 1,4 mL/min, whereas for elution it was less than 1 mL/min. The developed method was successfully applied to the separation and enrichment of trace Cu(II) in biological and natural water samples with satisfactory results. [source] Purification, crystallization and preliminary X-ray analysis of Mycobacterium tuberculosis folylpolyglutamate synthase (MtbFPGS)ACTA CRYSTALLOGRAPHICA SECTION F (ELECTRONIC), Issue 6 2006P. G. Young The gene encoding Mycobacterium tuberculosis FPGS (MtbFPGS; Rv2447c) has been cloned and the protein (51,kDa) expressed in Escherichia coli. The purified protein was crystallized either by the batch method in the presence of adenosine diphosphate (ADP) and CoCl2 or by vapour diffusion in the presence of ADP, dihydrofolate and CaCl2. X-ray diffraction data to approximately 2.0 and 2.6,Å resolution were collected at the Stanford Synchrotron Radiation Laboratory (SSRL) for crystals grown under the respective conditions. Both crystals belong to the cubic space group P213, with a unit-cell parameter of 112.6 and 111.8,Å, respectively. Structure determination is proceeding. [source] | ||||||||||