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1.
Summary A simple and specific HPLC method with coulometric detection was developed for the determination of 2′-acetyl erythromycin
and erythromycin in human plasma. Methyl tert-butyl ether was used as the extraction solvent after alkalization of plasma
samples. The plasma extracts were chromatographed on a reverse phase column using 4-component mobile phase. The manual sample
preparation procedure was modified so that it could also be applied to the robotic system (Zymate™ Laboratory Automation System). The linear range was 0.25–7.0 μg/ml. The quantitation limit for 2′-acetyl erythromycin and
erythromycin was 0.05 μg/ml. Equivalent manual and robotic sample preparation methods were used to analyze a large number
of plasma samples. 相似文献
2.
L. Kaila L. H. J. Lajunen P. Kokkonen 《Journal of Thermal Analysis and Calorimetry》1989,35(2):371-377
Thermal stability of the clodronic acid complex formed with sodium (Na2CCl2(HPO3)2 ·4H2O) was studied using both dynamic and isothermal thermogravimetric analyses as well as mass spectra. The thermal decomposition has two stages: dehydration and loss of two molecules of hydrogen chloride. Using the isothermal TG data the first step was found to be a phase-boundary reaction while the second step obviously cannot be described with just one reaction mechanism. The final residue of the dynamic TG analyses above 810 K was found to be sodium metaphosphate.
Zusammenfassung Sowohl mittels dynamischer und thermogravimetrischer Untersuchungen als auch and Hand von Massenspektren wurde die thermische Stabilität des mit Natrium gebildeten Säurekomplexes Na2CCl2(HPO3)2·4H2O untersucht. Die thermische Zersetzung vollzieht sich in zwei Schritten: Dehydratation und Verlust von zwei Molekülen HCl. Auf Grund der isothermen TG Angaben ist der erste Schritt eine Phasengrenzreaktion, während der zweite Schritt mit einem einzigen Reaktionsmechanismus nicht eindeutig beschrieben werden kann. Das Endprodukt der DTG Analyse oberhalb 810 K erwies sich als Natriummethaphosphat.
-Na2CCl2/HPO3/2·4H2O — , - . , , , . , , . 810 .相似文献
3.
Leyla Bitiş Sevda Süzgeç Ulaş Sözer Hasan Özçelik Josef Zapp Alexandra K. Kiemer Filiz Meriçli Ali H. Meriçli 《Helvetica chimica acta》2007,90(11):2217-2221
From the aerial parts of Delphinium buschianum Grossh ., collected in Turkey, a new diterpenoid alkaloid 1 , named budelphine, was isolated along with the known diterpenoid alkaloids karakoline ( 2 ), 18‐hydroxy‐14‐O‐methylgadesine ( 3 ), delsoline ( 4 ), lapaconidine ( 5 ), columbianine ( 6 ), 14‐benzoylneoline ( 7 ), and hetisine ( 9 ). The structure of 1 was established on the basis of 1H‐, 13C‐, DEPT, 1H,1H‐COSY, NOESY, HSQC, and HMBC NMR studies. 相似文献
4.
The capillary electrophoretic-mass spectrometric analysis (CE-MS) of catecholamines was optimized with coaxial sheath flow interface and electrospray ionization (ESI). The parameters studied included the sheath liquid composition and its flow rate, separation conditions in ammonium acetate buffer together with the ESI and cone voltages as mass spectrometric parameters. In addition, the effect of ESI voltage on injection as well as the siphoning effect were considered. The optimized conditions were a sheath liquid composition of methanol-water (80:20 v/v) with 0.5% acetic acid, with a flow rate of 6 microL/min. The capillary electrophoretic separation parameters were optimized with 50 mM ammonium acetate buffer, pH 4.0, to +25 kV separation voltage together with a pressure of 0.1 psi. The most intensive signals were obtained with an ESI voltage of +4.0 kV and a cone voltage of +20 V. The nonactive ESI voltage during injection as well as avoidance of the siphoning effect increased the sensitivity of the MS detection considerably. The use of ammonium hydroxide as the CE capillary conditioning solution instead of sodium hydroxide did not affect the CE-MS performance, but allowed the conditioning of the capillary between analyses to be performed in the MS without contaminating the ion source. 相似文献
5.
Nermin Meriç Cezmi Kayan Nevin Gürbüz Mehmet Karakaplan Nil Ertekin Binbay Murat Aydemir 《Tetrahedron: Asymmetry》2017,28(12):1739-1749
Metal-catalyzed asymmetric transfer hydrogenation is a powerful and practical method for the reduction of ketones to produce the corresponding secondary alcohols, which are valuable building blocks in the pharmaceutical, perfume, and agrochemical industries. Hence, a series of novel chiral β-amino alcohols were synthesized by chiral amines with regioselective ring opening of (S)-propylene oxide or reaction with (S)-(+)-2-hydroxypropyl p-toluenesulfonate by a straightforward method. The chiral ruthenium catalytic systems generated from [Ru(arene)(μ-Cl)Cl]2 complexes and chiral phosphinite ligands based on amino alcohol derivatives were employed in asymmetric transfer hydrogenation of ketones to give the corresponding optically active alcohols; (2S)-1-{[(2S)-2-[(diphenylphosphanyl)oxy]propyl][(1R)-1-phenylethyl]amino}propan-2-yldiphenylphosphinitobis[dichol-oro(η6-benzene)ruthenium(II)] acts an excellent catalyst in the reduction of α-naphthyl methyl ketone, giving the corresponding alcohol with up to 99% ee. The substituents on the backbone of the ligands were found to have a remarkable effect on both the conversion and enantioselectivity of the catalysts. Furthermore, this transfer hydrogenation is characterized by low reversibility under these conditions. 相似文献
6.
Bünyamin Ak Duygu Elma Nermin Meriç Cezmi Kayan Uğur Işık Murat Aydemir Feyyaz Durap Akın Baysal 《Tetrahedron: Asymmetry》2013,24(20):1257-1264
A new and versatile class of unsymmetrical ferrocenyl-phosphinite ligands possessing a stereogenic center has been prepared from commercially available, inexpensive aminoacids such as, d-, l-phenylglycine and d-, l-phenylalanine, through a concise synthetic procedure. These ligands are not very sensitive to air and moisture, and display good enantioselectivities in the ruthenium-catalyzed asymmetric transfer hydrogenation of acetophenone derivatives, in which up to 91% ee was obtained. A comparison of the catalytic properties of amino alcohols and other analogues based on a ferrocenyl backbone is also discussed briefly. The structures of these ligands and their corresponding complexes have been elucidated by a combination of multinuclear NMR spectroscopy, IR spectroscopy, and elemental analysis. 相似文献
7.
M. Isakov J. Kokkonen K. Östman V.-T. Kuokkala 《The European physical journal. Special topics》2016,225(2):231-242
In this paper, methods to produce rapid strain rate changes for strain rate sensitivity measurements in Split Hopkinson Bar arrangements are presented and discussed. Two different cases are considered: a strain rate change test within the high strain rate region in compression, and a tension test incorporating a large strain rate jump directly from the low strain rate region to high strain rates. The former method is based on the loading wave amplitude manipulation, while the latter method is based on the incorporation of a low strain rate loading device into a Tensile Split Hopkinson Bar apparatus. 相似文献
8.
The beta dose response and Optically Stimulated Luminescence (OSL) signal stability characteristics of human tooth enamel deproteinated by hydrazine reagent under blue photon stimulation are reported. Removal of the protein organic component of tooth enamel resulted in a higher OSL sensitivity and slower fading of OSL signals. The effect of chemical sample preparation on the enamel sample sensitivity is discussed and further steps to make this deproteinization treatment suitable for in vitro dose reconstruction studies are suggested. 相似文献
9.
Lokanathan R. Arcot Meri Lundahl Orlando J. Rojas Janne Laine 《Cellulose (London, England)》2014,21(6):4209-4218
Cellulose nanocrystals (CNC) were functionalized in aqueous media at the reducing, aldehyde ends of cellulose. CNC oxidation to produce carboxyl groups was followed by carbodiimide-mediated reaction to install thiol groups. The selectivity and extent of thiolation at the reducing ends was qualitatively confirmed by imaging (transmission electron microscopy) silver nanoparticles that tagged the CNC termini and by X-ray photoelectron spectroscopy, respectively. The adsorption of thiolated CNC onto gold surfaces as well as the viscoelastic property of the formed adlayer was investigated by using quartz crystal microgravimetry. The thiolated CNC chemisorbed on the surfaces were further analyzed for surface density and distribution by using atomic force microscopy. Overall we introduce a facile, mild asymmetric thiolation procedure as an efficient alternative to conventional reductive amination. 相似文献
10.
Merijs Meri R. Jablonskis I. Zicans J. Kalnins M. Bledzki A. K. 《Mechanics of Composite Materials》2004,40(3):247-252
Considering the wide applicability of polymeric composite materials, heterogeneous blends of poly(ethylene terephtalate) (PET) and polyethylenes of high and low densities (HDPE and LDPE, respectively) were investigated. Rheological (the flow-behavior index), mechanical (the yield strength and the Charpy impact strength), and morphological (crystallinity and the melting temperature) properties were detected for individual blend components and different blend compositions. A radiation treatment (-rays) was applied to improve certain characteristics of the heterogeneous blends. The results of this investigation show that the radiation modification can be successfully used to improve some physical properties of the PET-based blends and to choose individual blend components, optimum irradiation conditions, and desirable blend compositions, which allows producing materials with a predictable set of mechanical properties. 相似文献