毛细管电泳技术分离麻黄碱和伪麻黄碱

设计了一篇反映现代化学内容的高中化学教学材料.通过用氧化石墨烯修饰毛细管柱分离麻黄碱和伪麻黄碱的研究实例,介绍毛细管电泳技术分离手性对映体的基本原理,内容涉及分子的手性、分子间作用力、氢键等高中化学知识,供一线高中化学教师用于教学实践.     

区段灌注毛细管电泳研究药物与牛血清白蛋白的相互作用

以毛细管电泳为手段,采用毛细管区段灌注技术,对麻黄碱、咖啡因和扑热息痛3种药物与牛血清白蛋白(BSA)之间的相互作用进行了研究。将两个较短的药物区带分别置于一个较长的BSA区段前后,以区段前的药物为标记物,采用峰漂移模型,同时测得麻黄碱、咖啡因和扑热息痛与BSA的结合常数,其值分别为 3.38×104 L/mol , 4.79×104 L/mol 和 6.13 ×104 L/mol 。结果表明这种方法可作为药物与蛋白相互作用分析的一种改进方法,并且有效地避免了常规峰漂移模型和迎头分析法中     

Spectres RMN-13C DE β-Aminoalcools Derives DE L'Ephedrine ET De Leurs Oxazolidines

Abstract

The carbon-13 NMR spectra of β-aminoalcohols related to nor-and pseudonor-ephedrine (N-CH₃; N-C₂H₅; N-iC₃H₇; N-tC₄H₉) and the series of the corresponding oxazolidines from formaldehyde and benzaldehyde were obtained and dicussed. The configuration of the 3-alkyl-2, 5-diphenyl-4-methyloxazolidines was established.     

高效液相色谱法测定麻黄浸膏粉中麻黄类生物碱

采用高效液相色谱法分离了麻黄浸膏粉中去甲基麻黄碱、去甲基伪麻黄碱、麻黄碱、伪麻黄碱和甲基麻黄碱等 5种主要麻黄类生物碱。所用分离柱为HIQSILC18,流动相为含少量 (体积分数为 0 .2 % )甲醇的 0 .0 2mol L磷酸二氢钠溶液 (用HCl和三乙胺调至pH 3.2 )。 5种麻黄类生物碱在 2 5min内得到了有效分离、峰型对称且尖锐。     

毛细管电泳-方波安培法分离检测滴鼻液中的麻黄碱

在熔融石英毛细管 (75mm× 5 0cm )中 ,以 5mmol/LTris(三羟甲基氨基甲烷 ) +5mmol/LH3 BO3(pH =6 .5 )为电泳介质 ,采用毛细管电泳 方波安培检测法 ,实现了滴鼻液中盐酸麻黄碱的分离检测。探讨了缓冲溶液的种类、浓度、pH值、检测电位等因素对分离检测效果的影响。线性范围为 0 .8～ 2 0 2mg/L ,检出限为 0 .3mg/L ,回收率为 92 %～ 10 4 %。     

Micellar liquid chromatographic method for the determination of ephedrine and pseudoephedrine in human serum by direct inject of the sample with simple dilution

A micellar high-performance liquid chromatographic method was developed to simultaneously determine ephedrine and pseudoephedrine in human serum. The serum sample pretreatment was a simple dilution in a micellar solution, filtration, and direct injection, thus avoiding time-consuming and tedious steps. Hence, there is no need to use an internal standard. The serum samples were analyzed using a mobile phase containing 1.50?×?10^?1?mol/L sodium dodecyl sulfate and 0.02?mol/L sodium dihydrogen phosphate with 7.5% (v/v) 1-propanol at pH 3.0, running at 1.0?mL/min by an Inertsil C18 (150?×?4.6?mm, 5?µm) column at 30°C. The UV wavelength was set at 210?nm. The developed method was validated by linearity (r?>?0.9990) and intra- and inter-day precisions of ephedrine and pseudoephedrine (relative standard deviation; RSD%, 0.04–10.40, and RSD %, 0.30–10.25, respectively), LODs for ephedrine and for pseudoephedrine was 2.63 and 2.70?µg/mL, respectively; lower limit of quantification for ephedrine and for pseudoephedrine was 4.38 and 4.51?µg/mL, respectively. Finally, the proposed method was applied to investigate ephedrine and pseudoephedrine in real human serum samples after oral administration of Kechuanning Koufye including Ephedra herb. It is environmentally friendly, easy-to-handle, and feasible method for routine analysis in clinical laboratory.     

Continuous capillary electrophoresis with flow injection and its application for determination of Ephedrine and Pseudo-ephedrine in Chinese medicinal preparations

This article presents a new, simple and rapid continuous separation method by combination of flow injection with capillary electrophoresis designed for the analysis of basic traditional Chinese medicines. The device was produced using commercial capillary and components readily available in analytical laboratory. In double-T configuration, the designed horizontal separation channel was 25 microm i.d. x 146 mm length (an effective separation length of 93 mm) quartz capillary, with two vertical elicitation arms produced from 0.5 mm i.d. pump tubing. The capillary was embedded in a 40 x 20 x 3 mm organic glass base. Using the double-T configuration, continuous introduction of a series of samples was achieved. More than 3.00 resolution for ephedrine and pseudo-ephedrine were obtained using 100 mm borate buffer (pH 9.80) within 8 min in 25 microm separation channel with an electrical field strength of 137 V/cm (UV detection at 215 nm). The linear calibration range was 50-1500 microg/mL (ephedrine, r = 0.9982; pseudo-ephedrine, r = 0.9990) for both analytes. The limits of detection were 2.65 micro g/mL for ephedrine and 2.92 microg/mL for pseudo-ephedrine. In this device, the contents of ephedrine and pseudo-ephedrine in five Chinese medicinal preparations were determined with RSDs (n = 5) in range 1.16-4.51% and recoveries in range 90.4-114.6%.     

二阶导数光谱测定呋麻滴鼻液中盐酸麻黄碱的含量

本文采用二阶导数光谱法，测定呋麻滴鼻液中盐酸麻黄碱的含量，排除了呋喃西林的干扰，方法简单，快速，准确。平均回收率为９９．５％（ｎ＝８），ＳＤ＝０．７３，ＣＶ＝０．７３％。\     

麻黄碱衍生噁唑烷类化合物的立体选择性合成

麻黄碱衍生噁唑烷类化合物是由麻黄生物碱和醛酮缩合而成的杂环化合物，它既比相应的麻黄碱碱性弱，脂溶性高，又比相应的醛、酮理化性质稳定，是比较有前途的麻黄碱类前体药物。我们利用麻黄生物碱和取代苯甲醛，立体选择性地合成出十一种噁唑烷类化合物(图1)。     

Effect of Doping Silica Gel Layers with TiOTi-Chains and Cu2+-Ephedrine on the Sensitivity of the Layers to Gases

In this paper the interaction of polysiloxane and TiOTi-doped polysiloxane gel layers containing Cu²⁺-ephedrine (CuEP) with carbon dioxide, nitrogen and water is investigated. This interaction is studied through changes of the output optical power from an optical fiber coated with the investigated gel layer. The layers are prepared with sols based on tetraethoxysilane and titanium isopropoxide, isopropanol, acetylacetone and Cu²⁺-ephedrine by the repeated dip-coating method. The applied gel layers are dried at 70°C.Spectral and temporal changes of the output optical power due to effect of the tested gases are measured. The measurements show big changes of the output optical power of fibers coated with CuEP-doped silica gel layers in a wavelength range from 400 to 700 nm, which is in relation with spectral effects of CuEP in alcoholic solutions. Relatively lower changes of the attenuation spectra without any attenuation band are found in the spectra of TiOTi-doped siloxane gel layers containing CuEP. The angular distributions of the output optical power of the coated fibers indicate high optical losses of the layers.