紫外分光光度法测定黄藤素注射液中盐酸巴马汀含量的探索

采用紫外分光光度法测定黄藤素注射液中盐酸巴马汀的含量,同时与药典方法进行比较,两者无显著差异。试验结果表明,该方法简便,快捷,灵敏度高,重现性好,可用于黄藤素注射液成品或半成品中盐酸巴马汀含量的快速测定和质量控制。     

Colorimetric and Bromometric Determination of Pirbuterol Hydrochloride

Abstract

Two proposed methods are reported for the quantitation of pirbuterol hydrochloride, namely, (i) colorimetric and (ii) titrimetric methods. The colorimetric method is based on coupling betweem diazotized sulphanilamide and pirbuterol hydrochloride. Under the optimum conditions studied, the coupling product exhibits a maximum at 440 nm. Linear relation between absorbance, A, and concentration of pirbuterol hydrochloride is in the range 5–40 μgml^?1. The mean percentage obtained for capsules (Exirel^R ?15 mg) was 100.8 ± 0.7 whereas mean percentage recovery obtained for the authentic drug was 100.5 ± 0.8.

The titrimetric procedure involves bromination of authentic pirbuterol in acid medium and residual titration of excess bromine. The stoichiometry of the reaction was investigated and infra-red analysis, of the bromoderivative was carried out. When applied to capsules the bromometric method gave mean percentage of 100.18 ± 2.25.     

纳米Ag/TiO_(2)纳米管阵列基底构建及表面增强拉曼散射光谱检测与降解盐酸四环素北大核心CSCD

将阳极氧化与光还原法结合,在TiO_(2)纳米管阵列(TiO_(2)NTAs)表面修饰Ag纳米粒子,获得一种均匀有序、稳定性高且可循环的TiO_(2)NTAs/Ag活性基底。采用X射线粉末衍射(XRD)、X射线光电子能谱(XPS)、紫外可见漫反射光谱(UV-Vis DRS)、表面增强拉曼散射光谱(SERS)和扫描电子显微镜(SEM)等手段对TiO_(2)NTAs/Ag的组成和结构进行了表征。进一步研究了该TiO_(2)-NTAs/Ag阵列对盐酸四环素(TC-HCl)的SERS响应,结果表明,该复合基底对TC-HCl具有较高的检测灵敏度,在水中检测限可达1×10^(−14) mol/L,而TiO_(2)-NTAs与Ag之间的协同效应对其检测性能的提高起着关键作用。此外,TiO_(2)NTAs/Ag基底在光照下对TC-HCl展示了优异的降解活性,且至少可循环使用8次。表明该TiO_(2)NTAs/Ag基底在环境中有机污染物的SERS检测和降解领域具有潜在的应用前景。     

Preparation and fabrication of porous-Fe2O3/carbon black nanocomposite: a portable electrochemical sensor for psychotropic drug detection in environmental samples

Herein, we reported the fabrication of porous iron oxide/carbon black (P–Fe₂O₃/CB) composite through a two-step engineering method. At first, Prussian blue microcubes were used as a precursor and further calcined to form P–Fe₂O₃ microcubes. The intercalation of CB nanoparticles with P–Fe₂O₃ nanocubes was processed through the ultrasonication method. The obtained P–Fe₂O₃/CB were successfully scrutinized through various physiochemical characterization methods. The proposed P–Fe₂O₃/CB-modified glassy carbon electrode sensor was successfully implemented in the electrochemical sensing of chlorpromazine hydrochloride due to its very low charge transfer resistance (R_ct) compared to the other electrode modifiers. The sensitive detection of CPMH through differential pulse voltammetry exemplifies an excellent electroanalytical performance such as a wide linear range of 0.5–1472 μM, a lower detection limit (0.001 μM), and an appraisable sensitivity of 1.99 μA/μM cm^?2 due to its availability of a high number of active sites and its large surface area, respectively. It also expresses excellent selectivity, repeatability, reproducibility, and stability results. Moreover, the practical feasibility of the as-fabricated P–Fe₂O₃/CB/glassy carbon electrode sensor shows exquisite recovery (98.1–100.8%) results with an appraisable current response in various biological, pharmaceutical, and environmental samples.     

Optimized POCl3-assisted synthesis of 2-amino-1,3,4-thiadiazole/1,3,4-oxadiazole derivatives as anti-influenza agents

Although recent decades have witnessed the synthesis of 1,3,4-thiadiazoles via phosphorus POCl₃-promoted cyclization reaction, simultaneous access to 2-amino-1,3,4-thiadiazole and 2-amino-1,3,4-oxadiazole analogs remains unexpected and elusive. Herein, a detailed regiocontrolled synthesis of 2-amino-1,3,4-thiadiazoles in good to high yields with good regioselectivities from readily available thiosemicarbazides using POCl₃ was disclosed. Meantime, to establish a comprehensive structure–activity relationship, 2-amino-1,3,4-oxadiazole derivatives as single regioisomers were prepared via EDCI·HCl-triggered cyclization of the thiosemicarbazide intermediates. The in vitro anti-influenza assays proved that the selected compounds with the pyrazine/pyridine ring exhibited certain inhibitory activities against influenza A virus strains A/HK/68 (H3N2) and A/PR/8/34 (H1N1) in MDCK cells. Among them, N-(adamantan-1-yl)-5-(5-(azepan-1-yl)pyrazin-2-yl)-1,3,4-thiadiazol-2-amine (4j) was the most active compound, and exhibited favorable activity with EC₅₀ values of 3.5 μM and 7.5 μM, respectively. In addition, the molecular docking results explained the reason why compound 4j had dual inhibitory activity and revealed the reasonable binding mode of this compound with the M2-S31N and M2-WT ion channels. This compound had the potential to be further developed as an anti-influenza drug.     

Stability study and quantitative determination of mebeverine hydrochloride in tablets by means of reversed-phase high-performance liquid chromatography

Summary A rapid and specific reversed-phase high-performance liquid chromatographic method (RPHPLC) is described for the determination of mebeverine hydrochloride in tablets. Elution was performed on an octyl silane column with a methanol-water mixture (75-25), containing 0.05% hexylamine as silanol-blocking agent, adjusted to pH 5.0 with phosphoric acid. The method gave accurate, precise and reproducible results. The mean recovery of the drug from six synthetic tablet mixtures was 100.0% with a relative standard deviation (RSD) of 0.94%. In order to test the specificity of the method, the interference of the degradation compounds of mebeverine hydrochloride and of the intermediates from the synthesis was investigated. None of them did interfere. By means of mass spectrometry and UV-spectrophotometry, the degradation compounds of mebeverine were identified as veratric acid and as 4-|ethyl-[2-(4-methoxyphenyl)-1-methylethyl]amino| 1-butanol. The stability study proved that mebeverine hydrochloride is very stable in tablets; the tablets still contain more than 95% of the declared drug potency after storage for more than one year at 50°C.Colofac; Duspatal; Duspatalin     

DSC study of cold and heat denaturation processes of β-lactoglobulin A with guanidine hydrochloride

The cold and heat denaturations of bovine P-lactoglobulin A ((β-lg A) has been studied in solutions of guanidine hydrochloride (GuHCI) by differential scanning calorimetry (DSC). The experimental results are presented and discussed. It is shown that the number of protons bound by the monomeric molecules of β-lg A was unchanged before and after its heat denaturation below pH 3, and that the activation energy of the heat denaturation was depressed owing to the presence of GuHCI. In the solutions with 2.50 and 3.06 mol/L of GuHCI, both the cold and heat denaturations of P-lg A were observed. In comparison with the heat denaturation, the activation energy of cold denaturation was far lower and the number of GuHCl molecules bound by the unfolded polypeptide chains after culd denaturation increased a lot. The absolute value of the enthalpy of cold denaturation was larger than that of heat denaturation. It was found by the analysis that the contribution to the total denaturational enthalpy of conformational change itself of the monomeric molecules of β-lg A was the lowest among the globulins, according to the average of the number of heavy atoms. Project supported by the National Natural Science Foundation of China, and by the fund for excellent items under Director of the Institute of Chemistry.     

Assay of cisapride in pharmaceutical formulations by visible spectrophotometry

Three spectrophotometric methods (A-C) for the assay of cisapride (CPD) in pure and dosage forms are described. Method A is based on the oxidative coupling reaction of CPD with 3-methyl-2-benzothiazolinone hydrazone hydrochloride (MBTH) in the presence of ferric chloride to form a coloured species (_max; 565 nm.) Method B is based on the oxidation of CPD with Fe (III) and subsequent chelation of Fe(II) to form a coloured complex with 1,10-phenanthroline (_max: 520 nm). Method C is based on the formation of a coloured charge-transfer complex between CPD and chloranilic acid (_max; 555 nm). Regression analysis of Beer-Lambert plots showed good correlation in the concentration ranges 2.0–32.0, 0.4–6.4 and 25.0–450.0 g/ml for methods A,B and C, respectively. The validity of the proposed methods was tested by analysing pharmaceutical dosage forms containing CPD and the relative standard deviations were within 1.0%     

Viscosities of poly(N-vinylacetamide) solutions in the presence of salts, urea and guanidine hydrochloride

Summary  In the aqueous solutions of poly(N-vinylacetamide) in the presence of Na₂SO₄ or (NH₄)₂SO₄, the intrinsic viscosities were small and the Huggins constants were large compared with those in water. Similar but much less effects were observed for NaF. Opposite effects were found, however, for NaSCN. The poor solvent quality of aqueous sulfate solutions was significantly improved by the addition of guanidine hydrochloride to 3 M or higher. Urea was much less effective in improving the solvent quality. The different M28.8neffects observed between urea and GdnHCl may be explained by their different binding affinities to amide group. Solubilization of PNVA flocculates induced by the presence of 0.8 M Na₂SO₄ took place by adding urea to 1 M, although only small changes were detected in the viscosity behavior accompanying the addition of 1 M urea. Received: 12 June 1997 Accepted: 4 August 1997     

Voltammetric Analysis of Oxymetazoline Hydrochloride at Zeolite – Modified Carbon Paste Electrode in Micellar Medium

Simple, sensitive, accurate and inexpensive differential pulse (DPV) and square wave (SWV) voltammetric methods utilizing zeolite modified carbon paste electrode (ZMCPE) were developed for the determination of Oxymetazoline hydrochloride (OXM) in nasal drops. Various experimental parameters were optimized using cyclic voltammetry (CV). Calibration curves were linear over the concentration ranges 9.8×10⁻⁸–3.6×10⁻⁶ M and 9.8×10⁻⁶–9×10⁻⁵ M for DPV and SWV, respectively. The DPV method showed a limit of detection (LOD) of 1.04×10⁻⁷ M. The method was applied for the determination of OXM in pharmaceutical formulation with an average recovery of 101.18 % (%RSD=0.41, n=9).