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111.
Summary A new, highly sensitive and selective gas chromatography method, using radiochemical detection (GC-DR) was developed for the
selective determination of3H-labelled deramciclane and its N-desmethyl metabolite in dog plasma. Inter-day accuracy and precision, as well as system
suitability of the GC-RD method was investigated during the method validation. The calibration curve was proved to be linear
(r=0.9986) in a wide concentration range (13–1000 ngeqv mL−1)
The lower limit of quantitation (LLOQ) was 13.7 ngeqv mL−1, and the limit of the detection (LOD) was 1 ngeqv mL−1.
Using this new GC-RD method, plasma levels of3H-labelled deramciclane and its metabolite were determined in dogs, after the administration of a single 10 mg kg−1 oral dose. Pharmacokinetic curves and the calculated pharmacokinetic parameters were compared to those obtained using a previously
elaborated gas chromatography-nitrogen selective detection method (GC-NPD) and to those obtained by measuring the plasma level
of total radioactivity (liquid scintillation counting, LSC). Pharmacokinetic curves and the calculated pharmacokinetic parameters
obtained with the two different gas chromatography detection methods (NPD and RD) showed good correlation. Comparison of these
results to those acquired by total radioactivity measurement demonstrated that deramciclane was intensively metabolised. Moreover,
the biological half-life (t
1
2/β
) of the unknown metabolites proved to be more than a magnitude longer than the half-life of the parent compound or that of
N-desmethyl metabolite.
Presented at: Balaton Symposium on High-Performance Separation Methods, Siófok, Hungary, September 3–5, 1997. 相似文献
112.
Polyethylene glycols can be immobilized in glass capillary columns by a new procedure involving covering the glass walls with a layer of graphitized carbon black and by flowing a mixture of the stationary phase and dicumyl peroxide. After curing and conditioning the column is ready for use. Excellent performance is reported for Carbowax 20 M and high molecular weight glycols. For other glycols the immobilized layer is less stable and can be washed out. 相似文献
113.
Most of the common classes of organic compounds chromatograph normally on Superoxes. There is no tailing or adverse effect from excessively different activity different activity coefficients. Superoxes are therefore universal phases for gas chromatography. This is also expressed by a wide useful temperature range from ~50° to ~300°. High MW Superox-4 has a MAOT about 20° higher than the lower MW Superox-0.1. Several applications illustrating the versatility of Superox phases in (GC)2 are presented. 相似文献
114.
K. H. Kim J. H. Lee M. Y. Ko K. S. Shin J. S. Kang W. C. Mar J. R. Youm 《Chromatographia》2002,55(1-2):81-85
Summary A method for the assay of R-(+)- and S-(−)- metoprolol in human urine has been developed using gas chromatography-mass spectrometry.
The method involved purification by liquid-liquid extraction and derivatization with N-methyl-N-(trimethylsilyl)trifluoroacetamide
to form an O-silyl ether, followed by subsequent chiral derivatization with (−)-α-methoxy-α-(trifluoromethyl)phenylacetyl
chloride to form diastereomeric amide. The reaction was rapid and the diastereomeric derivatives were well resolved. Quantitation
was performed by selected-ion monitoring of fragment ions of the diastereomers in electron impact ionization mode. No racemization
was found during the reaction. The detection limit was 0.5 ng·mL−1. The intra-day variation ranged between 0.38 and 7.86% in relation to the measured concentration and inter-day variation
was 2.26–8.06%. The method has been applied to the determination of R-(+)-and S-(−)- metoprolol in human urine from healthy
volunteers dosed with racemic metoprolol tartrate. 相似文献
115.
The effects of polymer chain rigidification, zeolite pore size and pore blockage on polyethersulfone (PES)-zeolite A mixed matrix membranes 总被引:1,自引:0,他引:1
Yi Li Tai-Shung Chung Chun Cao Santi Kulprathipanja 《Journal of membrane science》2005,260(1-2):45-55
The polyethersulfone (PES)-zeolite 3A, 4A and 5A mixed matrix membranes (MMMs) were fabricated with a modified solution-casting procedure at high temperatures close to the glass transition temperatures (Tg) of polymer materials. The effects of membrane preparation methodology, zeolite loading and pore size of zeolite on the gas separation performance of these mixed matrix membranes were studied. SEM results show the interface between polymer and zeolite in MMMs experiencing natural cooling is better (i.e., less defective) than that in MMMs experiencing immediate quenching. The increment of glass transition temperature (Tg) of MMMs with zeolite loading confirms the polymer chain rigidification induced by zeolite. The experimental results indicate that a higher zeolite loading results in a decrease in gas permeability and an increase in gas pair selectivity. The unmodified Maxwell model fails to correctly predict the permeability decrease induced by polymer chain rigidification near the zeolite surface and the partial pore blockage of zeolites by the polymer chains. A new modified Maxwell model is therefore proposed. It takes the combined effects of chain rigidification and partial pore blockage of zeolites into calculation. The new model shows much consistent permeability and selectivity predication with experimental data. Surprisingly, an increase in zeolite pore size from 3 to 5 Å generally not only increase gas permeability, but also gas pair selectivity. The O2/N2 selectivity of PES-zeolite 3A and PES-zeolite 4A membranes is very similar, while the O2/N2 selectivity of PES-zeolite 5A membranes is much higher. This implies the blockage may narrow a part of zeolite 5A pores to approximately 4 Å, which can discriminate the gas pair of O2 and N2, and narrow a part of zeolites 3A and 4A pores to smaller sizes. It is concluded that the partial pore blockage of zeolites by the polymer chains has equivalent or more influence on the separation properties of mixed matrix membranes compared with that of the polymer chain rigidification. 相似文献
116.
P. Torline G. du Plessis N. Schnautz J. C. Thompson 《Journal of separation science》1979,2(10):613-616
A detailed method for the routine preparation of glass capillary columns is presented. The method consists of coating a glass tube with quartz powder prior to pulling the tube into a capillary. The inner surface of the capillary consists of an even distribution of quartz particles fused to the walls. This surface has been found readily deactivated by standard procedures and ideal for the preparation of thick-film glass capillary columns. The method has been thoroughly tested in two independent laboratories to ensure that the procedures described are reproducible. 相似文献
117.
Summary Dynamic headspace and simultaneous steam distillation-extraction techniques were used to isolate volatile components of Parmesan cheese. Identification of the substances was carried out by GC and GC-MS; 110 compounds were identified in the samples obtained using the headspace technique, 105 in the extracts; among them, about 50 compounds were isolated with both procedures. Mass spectral data showed evidence for a number of newly reported compounds such as 3-(methylthio)propanal, -tetradecalactone, 9-tetra-decenoic and 9-hexadecenoic acids. Mass spectra of some compounds are discussed and a comparison between the results obtained with the two sampling methods is given. 相似文献
118.
119.
The present paper describes constructional details and evaluations of an at-column injector for capillary GC. Injections were made via a sample loop on a 0.32 mm i.d. capillary column. Two rotary valves were employed to allow a wash of the sample loop and a backflush of the transfer line. Repeatability, calculated from absolute area counts for n-alkanes was between 0.3–1% RSD, for injected sample volumes between 5 and 100 μl. Promising results were also obtained with syringe-based injections on narrow bore (100 μ i.d.) columns. Repeatability on the basis of normalized area counts was in the order of 0.1–0.2% RSD, while solvent tailing was practically absent. 相似文献
120.
As an alternative to acid pretreated UCON and FFAP capillaries for the analysis of wide-boiling free fatty acid mixtures, OV-1 : FFAP phase mixtures were used on high-temperature silylated inert glass capillary columns. The HETP-carrier gas velocity curves, peak asymmetry factors, coating efficiency, gas phase and stationary phase contributions to the mass transfer resistance were determined for various OV-1 : FFAP ratios. Mixed-phase capillaries showed optimum performance at a 2 : 1 OV-1 : FFAP ratio. The thermal and long-term stability of OV-1-stabilized FFAP columns surpassed those of the UCON and pure FFAP reference column used. 相似文献