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41.
A high-performance liquid chromatographic method for the separation and determination of 18 alpha-glycyrrhetinic acid and 18 beta-glycyrrhetinic acid has been developed. Indomethacin was used as an internal standard. The drugs were separated on a reversed-phase column and detected by UV detection at a wavelength of 254 nm. Methanol-water-perchloric acid-ammonia (80:20:0.4:0.4, v/v) was used as the mobile phase at pH of 7.0-7.5. The detection limit of both compounds was 0.1 microgram/ml in rat plasma. The method was applied to pharmacokinetic studies of glycyrrhetinic acids in rats. The results suggest that the pharmacokinetics appeared to be non-linear in nature. 相似文献
42.
Serdar S. Celebi Gow-Jen Tsai George T. Tsao 《Applied biochemistry and biotechnology》1991,27(2):163-171
Immobilization of glucoamylase (EC 3.2.1.3) on Celite R649 bio-catalyst carrier for hydrolysis of maltose and maltodextrin has been investigated in both packed bed and recirculated batch reactors. The kinetics parameters on the hydrolysis of maltose were estimated from the packed bed reactor. It is found that this immobilized enzyme is as efficient as the soluble enzyme in catalyzing hydrolysis of maltose. However, it is less efficient than the soluble enzyme in hydrolyzing 30% (w/v) maltodextrin, giving a maximum dextrose equivalent (DE) value of 96.0% instead of 98.2%. 相似文献
43.
A new approach to a CD45 protein tyrosine phosphatase inhibitor, pulchellalactam, is described. The key step of the sequence involves addition and elimination of an enolic lactam in a single step and 70% yield, employing an organocuprate reagent. The resulting alpha,beta-unsaturated lactam could be condensed with isobutyraldehyde to produce Z-pulchellalactam or converted into siloxypyrrole, which was subjected to the BF(3) x Et(2)O-promoted coupling reaction with isobutyraldehyde to afford E-pulchellalactam after E1-cB elimination and TFA deprotection. This first total synthesis afforded Z-pulchellalactam in six steps and 32% overall yield from Boc-glycine. The same sequence of reactions could also be applied to the liquid- or solid-phase synthesis of trifunctionalized pulchellalactam derivatives. 相似文献
44.
Hsu CL Chang SJ Lin YR Tsai SY Chen IC 《Chemical communications (Cambridge, England)》2005,(28):3571-3573
Vertically well aligned P-doped ZnO nanowires were prepared on ZnO-Ga/glass templates at 550 degrees C by reactive evaporation without metal catalysts and the nanowires were found to be single crystalline with the würtzite structure, oriented in the c-axis direction; the P-doping shortened the physical lengths of the ZnO nanowires without changing their diameter, and furthermore, the introduction of P atoms resulted in a much weaker and broader ZnO band edge emission. 相似文献
45.
In this study, the cooling effect was applied to an evanescent wave type infrared (IR) chemical sensing method to effectively trap volatile organic compounds (VOCs), which have been absorbed in the hydrophobic film coated around the internal reflection element (IRE). The detection of VOCs in aqueous solutions was taken in the headspace of the aqueous solution. This method eliminates the long-term instability of hydrophobic film soaked in an aqueous solution and the potential spectral interference caused by the matrix of the aqueous solution. Thermal energy has been applied to the aqueous solution to assist in the evaporation of VOCs out of the aqueous matrix. By applying a cooling system to the IRE, the excess thermal energy can be removed leading to more stable IR signals. After examination of organic compounds with vapour pressure (Pv) ranging from 0.017 to 150 Torr, significant differences were found between IR signals from cooled and un-cooled systems. Because the thermal conductivity of the IRE used in IR detection is typically low; the efficiency in removing the thermal energy is limited. By heating the aqueous solutions to different temperatures, the IR signals showed that the sample temperature was limited to around 80 °C. The IR signal determination results for five different volatility organic compounds indicated that the optimal heating temperature was not necessary to match with the volatilities of organic compounds in cooling system. The linear regression coefficient (R2) of the standard curve for sample concentrations in the range 5-200 μg ml−1 was generally higher than 0.991 and the detection limit was around a few hundred ng ml−1, which was two to three times lower than that of un-cooled system. 相似文献
46.
To investigate the disposition of unbound cocaine in the rat blood, brain and bile, we demonstrate an in vivo multiple sampling microdialysis system coupled with liquid chromatography for cocaine assay and verified by tandem mass spectrometry. Three microdialysis probes were concurrently inserted into the jugular vein, bile duct and brain striatum of each anesthetized rat. After a period of 2 h post-surgical stabilization, cocaine (10 mg kg(-1)) was administered through the femoral vein. Separation of unbound cocaine from various biological fluids was applied to a reversed-phase C(18) column (250 x 4.6 mm I.D., 5 microm). The mobile phase consisted of acetonitrile--10 mm potassium dihydrogen phosphate buffer (25:75, v/v, pH 4.0) and 0.8% diethylamine at a flow rate of 1 mL min(-1). The UV detector wavelength was set at 235 nm. The results indicate that cocaine penetrates the blood--brain barrier with a rapid distribution. However, unbound cocaine in the bile dialysate was not detectable in the UV detection. We therefore use LC--tandem mass spectrometry to detect the bile fluid after cocaine administration (3 mg kg(-1), i.v.). The results indicate that cocaine goes through hepatobiliary excretion. 相似文献
47.
Investigation of the root extract of Antidesma pentandrum var. barbatum led to the isolation of seven new compounds, antidesmol ( 1 ), antidesmanins E ( 2 ) and F ( 3 ), antidesnone ( 4 ), antidesnol ( 5 ), barbatumols A ( 6 ) and B ( 7 ), together with 14 known compounds including sodium aristolochate‐I ( 10 ) and aristolochic acid‐I methyl ester ( 11 ). 相似文献
48.
Simultaneous determination of berberine in rat blood,liver and bile using microdialysis coupled to high-performance liquid chromatography 总被引:5,自引:0,他引:5
High-performance liquid chromatography coupled to microdialysis was used for the simultaneous determination of unbound berberine in rat blood, liver and bile for a pharmacokinetic study. Microdialysis probes were simultaneously inserted into the jugular vein toward the right atrium, the median lobe of the liver, and the bile duct of male Sprague-Dawley rats for biological fluid sampling after administration of berberine (10 mg/kg) through the femoral vein. Berberine and dialysates were separated using a Zorbax SB-phenyl column and a mobile phase comprised of acetonitrile-methanol-20 mM monosodium phosphate (pH 3.0) (35:20:45, v/v) together with 0.1 mM 1-octanesulfonic acid. The detection limit for berberine was 10 ng/ml. The concentration-response relationship was linear (r2 > 0.995) over the concentration range 0.05-50 microg/ml; intra-assay and inter-assay precision and accuracy for berberine fell within predefined limits. The disposition of berberine in the blood, liver and bile fluid suggests that berberine might be metabolized in the liver and undergo hepatobiliary excretion. 相似文献
49.
Tsai TH 《Journal of chromatography. A》2005,1073(1-2):317-322
Genistein, the major isoflavone in soybeans, has been shown to have a wide range of effects. We used an HPLC-UV combined with microdialysis method to detect unbound genistein in rat blood, brain and bile. Genistein dialysates were eluted with a mobile phase containing acetonitrile-water (40:60, v/v, pH 3.5 adjusted by 0.1% acetic acid). Samples were separated using a phenyl (5 microm) column maintained at ambient temperature. The UV detector wavelength was set at 259 nm. The flow rate was 1.0 m/min. The limit of quantitation for genistein was 50 ng/ml. The in vitro recoveries of genistein were 31 +/- 1, 13 +/- 1 and 59 +/- 4% in microdialysis probes of blood, brain and bile, respectively (n = 4). Inter- and intra-assay accuracy and precision of the analysis were less than 10% in the concentration ranges of 0.05-5.0 microg/ml. A small ratio of genistein penetrates the blood-brain barrier (BBB) and goes through hepatobiliary excretion after genistein administration (10 or 30 mg/kg, i.v.). The brain-to-blood (AUC(brain)/AUC(blood)) and bile-to-blood (AUC(bile)/AUC(blood)) distribution ratios were 0.04 +/- 0.01 and 1.85 +/- 0.42, respectively for the dosage of genistein 30 mg/kg. After co-administration of cyclosporine, a P-glycoprotein (P-gp) inhibitor, the distribution ratios of genistein in brain and bile were not significantly altered. These results suggest that the BBB penetration and hepatobiliary excretion of genistein may not regulated by P-gp. 相似文献
50.
Das C Berezovska O Diehl TS Genet C Buldyrev I Tsai JY Hyman BT Wolfe MS 《Journal of the American Chemical Society》2003,125(39):11794-11795
gamma-Secretase cleaves the transmembrane domain of the amyloid precursor protein, a process implicated in the pathogenesis of Alzheimer's disease, and this enzyme is a founding member of an emerging class of intramembrane proteases. Modeling and mutagenesis suggest a helical conformation for the substrate transmembrane domain upon initial interaction with the protease. Moreover, biochemical evidence supports the presence of an initial docking site for substrate on gamma-secretase that is distinct from the active site, a property predicted to be generally true of intramembrane proteases. Here we show that short peptides designed to adopt a helical conformation in solution are inhibitors of gamma-secretase in both cells and enzyme preparations. Helical peptides with all d-amino acids are the most potent inhibitors and represent potential therapeutic leads. Subtle modifications that disrupt helicity also substantially reduce potency, suggesting that this conformation is critical for effective inhibition. Fluorescence lifetime imaging in intact cells demonstrates that helical peptides disrupt binding between substrate and protease, whereas an active site-directed inhibitor does not. These findings are consistent with helical peptides interacting with the initial substrate docking site of gamma-secretase, suggesting a general strategy for the development of potent and specific inhibitors of intramembrane proteases. 相似文献