Methodik und Anwendung des Radioimmunoassays

1. Einleitung

2. Tracerdarstellung

3. Geuinnung von Antiseren

4. Methoden zur Trennung von freier und antikörpergebundener Radioaktivität

5. Analysengang

6. Spezifität

7. Empfindlichkeit

8. Anwendungsbeispiele

9. Literatur     

Modified Preparation of 99mTe-Iron Hydroxide Macroaggregate (99mTe-Fe-(OH)2MA)

A modified method for preparing ^99mTc-FHMA for pulmonary studies is elabrated. It includes a new antioxidant sodium metabisulphite. The optimum conditions for the reparation are given. A simple and rapid procedure with a yield more than 98% is described which eliminates a further purification step.     

中药炮制机理研究的思路与方法——以咖啡豆的烘焙原理研究为例

中药炮制是中药学的特色和优势,也是最具我国自主知识产权的学科之一.中药炮制研究的核心是阐明中药炮制机理,这也是制约中药现代化的关键节点.目前大部分中药的炮制机理尚不明确,有待进行系统深入的研究.咖啡豆需要烘培后才可以制成饮料,这个高温烘培过程类似于中药的炮制过程.近年来,国内外专家对咖啡豆高温烘培过程化学成分变化及其机理进行了深入研究,各种新方法和新技术得到广泛应用,取得了系列研究成果,这些研究成果为中药炮制机理研究提供了多种新思路和新方法,也为中药炮制机理的研究和阐明提供了重要示范.     

论卤盐养生（8）

卤盐（包括食盐）是中国矿物药的重要组成部分。从文化价值、临床应用和情志调摄3个方面诠释了卤盐的养生学意义,并全面、详细地阐述了食盐对中国古代文化的四大贡献、6种盐类的现代临床应用价值以及盐湖旅游的6项要素;列举了160多个盐湖卤水的主要化学成分、矿化度或微量元素;摘录了论述卤盐主治功用的古今文献。本文分期刊出。     

Screening of aromatase inhibitors in traditional Chinese medicines by electrophoretically mediated microanalysis in a partially filled capillary

An electrophoretically mediated microanalysis method with partial filling technique was developed for screening aromatase inhibitors in traditional Chinese medicine. The in‐capillary enzymatic reaction was performed in 20 mM sodium phosphate buffer (pH 7.4), and sodium phosphate buffer (20 mM, pH 8.0) was used as a background electrolyte. A long plug of coenzyme reduced β‐nicotinamide adenine dinucleotide 2′‐phosphate hydrate dissolved in the reaction buffer was hydrodynamically injected into a fused silica capillary followed by the injection of reaction buffer, enzyme, and substrate solution. The reaction was initiated with a voltage of 5 kV applied to the capillary for 40 s. The voltage was turned off for 20 min to increase the product amount and again turned on at a constant voltage of 20 kV to separate all the components. Direct detection was performed at 260 nm. The enzyme activity was directly assayed by measuring the peak area of the produced β‐nicotinamide adenine dinucleotide phosphate and the decreased peak area indicated the aromatase inhibition. Using the Lineweaver–Burk equation, the Michaelis–Menten constant was calculated to be 50 ± 4.5 nM. The method was applied to the screening of aromatase inhibitors from 15 natural products. Seven compounds were found to have potent AR inhibitory activity.     

A new strategy based on cholesterol-functionalized iron oxide magnetic nanoparticles for determination of polycyclic aromatic hydrocarbons by high-performance liquid chromatography with cholesterol column

This study reported for the first time the use of cholesterol-functionalized magnetic nanoparticles (Fe₃O₄@SiO₂@Chol) for the determination of polycyclic aromatic hydrocarbons (PAHs) in traditional Chinese medicine samples (TCMs) by high performance liquid chromatography (HPLC) coupled with fluorescence detection. The method was efficient, environmentally friendly, and fast. The solvent consumption of the proposed column is only half of the conventional column but with higher efficiency. Influencing factors, including sorbent amount, desorption solvent, sample volume and extraction time, were investigated in detail. Under the optimum conditions, good linearity (R² > 0.991) was obtained over the range of 5–400 ng g⁻¹, with limits of detection (LOD) 0.75, 0.50, 1.0, 0.56, 0.60, 0.84 and 0.80 ng g⁻¹ for anthracene, fluoranthene, pyrene, chrysene, benzo[a]anthracene, benzo(b)fluoranthene and benzo(k)fluoranthene, respectively.     

Quantitative analysis and pharmacokinetics study of tigecycline in human serum using a validated sensitive liquid chromatography with tandem mass spectrometry method

Tigecycline, a novel intravenously administered glycylcycline antibiotic, currently plays a key role in the management of complicated multiorganism infections. However, current liquid chromatography with tandem mass spectrometry methods briefly describe parameters and the only reported internal standard was sometimes difficult to obtain. In our study, an updated liquid chromatography with tandem mass spectrometry method for the quantitative analysis of tigecycline in human serum was developed. Sample preparation involved precipitation with 20% trichloroacetic acid. Chromatographic separation of tigecycline and tetracycline (internal standard) was achieved on a Hypersil GOLD C₁₈ column using gradient elution. The selected reaction monitoring transitions were performed at m/z 586.1→513.2 for tigecycline and m/z 445.1→410.2 for tetracycline. The assay was linear over the concentration range of 5–2000 ng/mL. The intra‐ and interday precisions at three concentration levels (10, 100, and 1600 ng/mL) were <15% and their accuracies were within the range of 95.1–106.1%. The mean recovery ranged from 94.3 to 105.6% and the matrix effect from 92.1 to 97.6%. Tigecycline was stable under all tested conditions. This validated method was successfully applied to a pharmacokinetic study in critically ill patients. The data demonstrated that our method allows quantification of tigecycline in serum in a quick and reliable manner for widespread application.     

Static headspace‐multicapillary column with gas chromatography coupled to ion mobility spectrometry as a simple approach for the discrimination of crude and processed traditional Chinese medicines

The processing procedure can alter the nature and chemical transformation of traditional Chinese medicine to accommodate different clinical dispensing and preparation requirements. In this study, static headspace‐multicapillary column with gas chromatography coupled to ion mobility spectrometry was developed for the rapid and sensitive discrimination of crude and processed traditional Chinese medicine. Using Radix Paeoniae Alba as a traditional Chinese medicine model, the combined power of this approach was illustrated by classifying the crude and processed Radix Paeoniae Alba samples into two main categories. The contents of the main components in Radix Paeoniae Alba varied significantly. The established method could promote the use of ion mobility spectrometry in intrinsic quality control and differentiation of herbal medicines from other processed products or preparations.     

线上线下混合式物理化学实验研究型教学改革

针对目前实验教学在创新型人才培养中存在的问题,介绍了北京航空航天大学化学学院物理化学实验教学的改革与实践情况。结合线上教学灵活、不受时空限制,以及线下教学培养学生动手操作能力和严谨求实的科学素养的特点,从递进式教学内容设计、个性化实验操作指导和训练、科研式论文报告总结、针对性展示和专题分析等方面进行了线上线下混合式研究型教学改革。将理论方法、虚拟操作、实际训练和总结提升等相结合,充分发挥教师指导和学生主体的优势,多维度培养和提升学生的科学素养、创新思维和综合创新能力,为提升实验教学质量和促进创新型人才培养提供了有益的借鉴。     

高效液相色谱-四极杆-飞行时间质谱快速筛查鉴别食品中非法添加的62种中药材北大核心CSCD

建立了高效液相色谱-四极杆-飞行时间质谱快速筛查鉴别食品中非法添加的62种中药材的方法。依据卫生部关于进一步规范保健食品原料管理的通知(卫法监发[2002]51号)中可用于保健食品的物品名单,确定食品中可能非法添加的62种中药材原料清单,再从62种中药材中筛选其特征组分,获得不同中药材对应的特征组分清单。62种对照药材经甲醇超声提取后,于Thermo Accucore aQ色谱柱(150 mm×2.1 mm,2.6μm)上分离,在电喷雾正负离子扫描模式下,分别以0.1%(v/v)甲酸水溶液-乙腈和水-乙腈为流动相梯度洗脱,进行一级质谱和二级质谱全扫描检测,采用Library View软件建立不同中药材对应的特征组分的一级精确质量数据库和二级碎片质谱库。样品同法处理后上样分析,采用Peak View软件将样品高分辨数据与自建数据库中的质谱图、精确分子离子质量数、碎片离子质量数、保留时间等相关参数进行快速筛查鉴别分析。该工作通过建立“中药材-特征组分”对应清单,构建了食品中易非法添加的62种中药材中共388种特征组分的高分辨质谱库,每种中药材包括5~10种特征组分,通过对实际食品样品配制酒、代用茶及饮料进行筛查分析,1批次配制酒样品与淫羊藿中药材的7种特征组分匹配一致,推断该配制酒样品中加入了淫羊藿中药材。该法可实现无标准品情况下中药材的定性筛查,具有高通量、准确、简便、快捷的特点,解决了食品中非法添加中药材难以识别和确证的难题,可以实现食品中非法添加中药材的快速筛查鉴别分析。