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51.
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53.
den Brok MW Nuijen B Miranda E Floriano P Munt S Manzanares I Beijnen JH 《Journal of chromatography. A》2003,1020(2):251-258
ES-285 x HCl [(2S,3R)-2-amino-3-octadecanol hydrochloride] is a novel investigational anticancer agent, which has shown in vitro and in vivo cytotoxic activity against various tumor cell lines with selectivity for certain solid tumors. The pharmaceutical development of ES-285 x HCl warranted the availability of an assay for the quantification and purity determination of ES-285 x HCl active pharmaceutical ingredient (API) and its pharmaceutical dosage form. A liquid chromatographic method (LC) comprising of derivatisation of ES-285 x HCl with phenylisothiocyanate and UV-detection was developed. The method was found to be linear, precise and accurate. The assay also proved selectivity as determined by analysing ES-285 x HCl in combination with 15 analogues and in combination with hydroxypropyl-beta-cyclodextrin, the excipient used in the lyophilised pharmaceutical dosage form. Stress testing showed that the degradation products were separated from the parent compound, confirming its stability indicating capacity. The method was found robust as determined with design of experiments (DoE), which made it possible to predict system suitability responses in worst case experimental conditions and to define criteria for system suitability testing. 相似文献
54.
Dissolved aluminium in seawater and freshwater is determined by cathodic stripping voltammetry (c.s.v.) preceded by adsorptive collection of complex ions with 1,2-dihydroxyanthraquinone-3-sulphonic acid (DASA) on the hanging mercury drop electrode. Complexation of aluminium by DASA is rapid and no waiting period or heating of the sample is required. Optimal conditions are a DASA concentration of 10?5 M, a solution pH of 7.1–7.3 and an adsorption potential of ?0.9 V; the c.s.v. scan is done in the differential-pulse mode. The limit of detection is 1 nM aluminium for an adsorption time of 45 s. The total time needed, including 50min deaeration and a standard addition, is 10–15 min per sample. No serious interferences were found; u.v. irradiation is recommended for samples containing high levels of organic materials. 相似文献
55.
56.
A simple, rapid and sensitive high-performance thin-layer chromatographic assay for the determination of epoxide hydrolase activity in rat liver homogenates is described. It is extended to the determination of a series of phenoxypropane-1,2-diols. The hydrolase assay has the advantages of using a readily available substrate, 2,3-epoxypropyl 4-methoxyphenyl ether, of multiple sample application, and of the simultaneous determination of reaction product (diol) as well as unchanged substrate (epoxide). The use of an internal standard, 4-nitroanisole, results in high sensitivity and good reproducibility of the proposed method. The limit of diol detection is 20 pmol. 相似文献
57.
Ester van den Beuken Sylvie Samson Elizabeth J. Sandoe G. Richard Stephenson 《Journal of organometallic chemistry》1997,530(1-2):251-253
The first example of an alkyne-substituted tricarbonyl(η5-cyclohexadienyl)iron(1+) complex has been prepared and the ω directing effect of the phenylethynyl substituent has been demonstrated in nucleophile addition reactions. Addition of NC− also occurs at the a position to form an unusual η1, η3-structure. 相似文献
58.
Thermal Properties of Hot-Stage Extrudates of Itraconazole and Eudragit E100. Phase separation and polymorphism 总被引:1,自引:0,他引:1
Six K. Leuner Ch. Dressman J. Verreck G. Peeters J. Blaton N. Augustijns P. Kinget R. Van den Mooter G. 《Journal of Thermal Analysis and Calorimetry》2002,68(2):591-601
Solid dispersions of itraconazole and eudragit E100 were prepared by hot-stage extrusion. Analysis of the physical structure
revealed the existence of different phases, depending on the manufacturing condition. Extrudates prepared at 453 K existed
as a molecular dispersion of itraconazole in eudragit E100 when the drug concentration did not exceed ca. 13% mass/mass. At
higher concentrations, a second phase consisting of pure glassy itraconazole emerged. In other dispersions prepared at 413
K, the second phase consisted of pure crystalline itraconazole. The difference can be attributed to the relation of the process-temperature
to the melting point. Heating of both dispersions induced cold crystallization. Extrudates prepared at 453 K showed comparable
behavior before and after milling, with the exception that unmilled dispersions with a drug load of ≥60% mass/mass recrystallized
upon heating into a polymorphic modification of itraconazole (T
m=431 K). Upon further heating the polymorph recrystallized to the stable crystalline form (T
m=441 K).
This revised version was published online in August 2006 with corrections to the Cover Date. 相似文献
59.
V. V. Barbakadze E. P. Kemertelidze I. Targamadze K. Mulkidzhanyan J. Kemink A. J. J. van den Berg K. J. Beukelman A. I. Usov 《Chemistry of Natural Compounds》2005,41(4):374-377
Two high-molecular-weight (>1000 kDa) water-soluble preparations were isolated from stems of Symphytum asperum and S. caucasicum. Their basic component was established as poly[hydroxy-1-carboxy-2-(3,4-dihydroxyphenyl)ethylene], analogous to that of high-molecular-weight
(>1000 kDa) preparations from roots of these same plants, using IR and NMR spectral data.
__________
Translated from Khimiya Prirodnykh Soedinenii, No. 4, pp. 303–305, July–August, 2005.
An erratum to this article is available at . 相似文献
60.
Tiggelaar RM Berenschot JW de Boer JH Sanders RG Gardeniers JG Oosterbroek RE van den Berg A Elwenspoek MC 《Lab on a chip》2005,5(3):326-336
In this paper the fabrication and electrical characterization of a silicon microreactor for high-temperature catalytic gas phase reactions, like Rh-catalyzed catalytic partial oxidation of methane into synthesis gas, is presented. The microreactor, realized with micromachining technologies, contains silicon nitride tubes that are suspended in a flow channel. These tubes contain metal thin films that heat the gas mixture in the channel and sense its temperature. The metal patterns are defined by using the channel geometry as a shadow mask. Furthermore, a new method to obtain Pt thin films with good adhesive properties, also at elevated temperatures, without adhesion metal is implemented in the fabrication process. Based on different experiments, it is concluded that the electrical behaviour at high temperatures of Pt thin films without adhesion layer is better than that of Pt/Ta films. Furthermore, it is found that the temperature coefficient of resistance (TCR) and the resistivity of the thin films are stable for up to tens of hours when the temperature-range during operation of the microreactor is below the so-called "burn-in" temperature. Experiments showed that the presented suspended-tube microreactors with heaters and temperature sensors of Pt thin films can be operated safely and in a stable way at temperatures up to 700 degrees C for over 20 h. This type of microreactor solves the electrical breakdown problem that was previously reported by us in flat-membrane microreactors that were operated at temperatures above 600 degrees C. 相似文献