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101.
P. Guinebault C. Dubruc A. Haddouche C. Colafranceschi G. Bianchetti 《Chromatographia》1988,26(1):377-382
Summary In order to follow levels of S-Carboxymethyl-L-cysteine in biological fluids for a period as long as three half-lives after drug administration during pharmacokinetic studies, an improved method for its determination had to be developed. Like the previous one, this method uses a protein precipitation step followed by an O-Phthalaldehyde derivatization step and then an HPLC on-line clean-up. This latter was obtained by means of a switching valve system, including a Nucleosil CN 5 m (3 cm × 4.6 mm i.d.) precolumn and a Spherisorb ODS 5 m (15 cm×4.6 mm i.d.) analytical column. The sensitivity limit was improved to 0.1 g/ml in plasma samples and 0.2 g/ml in urine samples.This method was applied in studies comparing single (0.75 g) and repeated (0.75 g tid) oral administration of the drug to 30 elderly patients and 20 healthy volunteers. Results showed that the half-life was 40% longer in elderly patients than in healthy volunteers, and that area under the plasma concentration versus time curve (AUC) values in elderly patients were twice those obtained with young subjects. 相似文献
102.
A PVC membrane vanadyl (VO2+) ion-selective electrode was constructed using 1,8-diaminonaphthalen (DAN) as a neutral carrier. The electrode shows good Nernstian response for VO2+ ions over a wide concentration range (1.0×10−1-1.0×10−5 M). The optimum composition of the membrane was 55 wt.% poly(vinylchloride), 35 wt.% 2-nitrophenyl octyl ether (NPOE), 5 wt.% ionophore, and 5 wt.% potassium tetrakis(p-chlorophenyl)borate (KTpClPB). It has relatively fast response time and can be used at least for 5 weeks without any considerable divergence in potentials. The proposed electrode revealed relatively good selectivity for VO2+ over wide variety of other metal ions. The electrode was used for the potentiometric titration of VO2+ ions with EDTA. 相似文献
103.
A selective, sensitive, and accurate high-performance liquid chromatographic method for determination of diltiazem in plasma samples has been developed and validated. The effects of mobile phase composition, buffer concentration, mobile phase pH, and concentration of organic modifiers on retention of diltiazem and internal standard were investigated. Solid-phase and liquid–liquid extraction were examined and proposed for isolation of the drug and elimination of endogenous plasma interferences. A 5 m Lichrocart Lichrospher 60 RP-select B chromatographic column was used; the mobile phase was acetonitrile–0.025 mol L–1 KH2PO4 (pH 5.5), 35:65 ( v / v) at a flow-rate of 1.5 mL min–1. The detection wavelength was 215 nm. The calibration plots were linear in the concentration range 20.0–500.0 ng mL–1. The method has been implemented to monitor diltiazem levels in patient samples. 相似文献
104.
胱氨酸(Cystine,Cys)在碱性条件下与新生成的ZnS悬浮液反应,生成可溶性碱式胱氨酸锌配合物,再用塞曼原子吸收光谱测定溶液中的总锌浓度即可间接的得到胱氨酸的含量.优化了测定的条件,在pH 9.40的2%硼砂底液中于室温下,使胱氨酸试液与新生成的ZnS悬浮液反应20min,离心分离后测定上层清液锌的FAAS响应.在所选定的条件下胱氨酸测定的线性浓度范围为0-450μg·mL-1,特征浓度为4.40μg·mL-1,检出限为4.20μg·mL-1.该法用于样品中的胱氨酸测定,其相对标准偏差RSD为4.45%(n=7),方法的回收率在70.8%-105.8%之间.并对测定机理进行了探讨. 相似文献
105.
106.
Summary A method has been developed for the extraction and rapid analysis of D-glaucine inGlaucium flavum Crantz. Simple extraction of the drug with diethyl ether was followed by high-performance liquid chromatography on a μBondapak C18 column using a mixture of acetonitrile, methanol and phosphate buffer as the mobile phase. Data on selectivity, sensitivity
and precision demonstrate the reliability of this method. 相似文献
107.
108.
Eberhard Reimann Wolfgang Erdle Eugen Hargasser Hermann Lotter 《Monatshefte für Chemie / Chemical Monthly》2002,133(7):1017-1030
Summary. The stereoselective synthesis of cis-ergoline is presented. Starting from rac-N-benzoyl tryptophan methyl ester, the key compound indolinylmethylpyridin-3-one was prepared via a seven-step reaction in good yield. Since its cyclization to the desired ergolinone failed, the key compound was reduced
to yield the two diastereomeric pyridin-3-ols; only one of them cyclized in trifluoromethanesulfonic acid, affording cis-ergoline. Catalytic hydrogenation of the latter gave N,N′-dimethyldihydroergoline, the X-ray crystallography of which revealed both the correct structure and identical relative configurations
at C-5a and C-6a (SS or RR). Hydroboration and subsequent perruthenate oxidation of the Δ9-ergoline provided access to the regioisomeric ergolinols and ergolinones.
Received December 27, 2001. Accepted January 15, 2002 相似文献
109.
Summary The adduction constants for the following eight binary systems were measured by gas liquid chromatography, at different temperatures: tetrachloromethane/p-xylene, tetrachloromethane/pseudocumene, chloroform/p-xylene, chloroform/pseudocumene, chloroform/aniline, m-methylphenol/aniline, o-methylphenol/aniline, and o-chlorophenol/aniline. The relationships between the adduction constant and temperature were used to fit the enthalpies and entropies of adduct formation. 相似文献
110.
电热原子吸收法测定人发中硒时不同改进剂的研究 总被引:2,自引:0,他引:2
对于生物体中硒的测定,国内外已有大量报道,所用方法也相当广泛。本文利用石墨炉原子吸收对人发中硒的测定进行了研究;对使用较多的两种硒的基体改进剂:铜与镍的作用与效果进行了研究,发现铜较镍在某些方面更为优越。当选用100 μg/mL的铜作改进剂时,硒的特征浓度为0.13 ng/1%abs,测定精度为3.4%~5.4%;线性范围达400 ng。 相似文献