毛细管电泳安培检测法在中草药分析中的应用

由于毛细管电泳安培检测法（CE-AD）具有高的分离效率和低的检测限的优势，现已在分析科学的各个领域，特别是在药物行业中得到广泛应用。中草药的研究在我国医药事业中占有重要的地位，采用CE-AD分离并检测中草药中有效成分对于促进中草药的药理药效研究及中草药的定量分析和质量监测等有重要意义。本文综述了CE-AD在中草药及中药复方制剂中有效成分分析中的应用，评述了该法与其他分离分析方法相比在中草药分析中的优越性，并对CE-AD在中草药分析中的发展进行了展望。     

毛细管电泳安培检测法在中草药分析中的应用

由于毛细管电泳安培检测法(CE-AD)具有高的分离效率和低的检测限的优势,现已在分析科学的各个领域,特别是在药物行业中得到广泛应用.中草药的研究在我国医药事业中占有重要的地位,采用CE-AD分离并检测中草药中有效成分对于促进中草药的药理药效研究及中草药的定量分析和质量监测等有重要意义.本文综述了CE-AD在中草药及中药复方制剂中有效成分分析中的应用,评述了该法与其他分离分析方法相比在中草药分析中的优越性,并对CE-AD在中草药分析中的发展进行了展望.     

芯片毛细管电泳-安培检测系统

由于安培检测具有的高灵敏度、低成本、低能耗、易集成化便携化、与微加工技术匹配等特点,芯片毛细管电泳-安培检测系统（μCE-AD）的研究近年来得到人们广泛的关注。本文结合本课题组的研究工作,对近年来μCE-AD的研究进展进行评述;重点讨论了近年来在芯片的设计、集成化电极的制备、消除分离电压的干扰等方面的进展;同时介绍了利用分离电场拓展检测范围、阵列电极和阵列通道、化学修饰电极的应用、新型进样技术和试样预处理等方面的新成就;最后展望了未来μCE-AD的发展趋势。     

离子色谱在中草药成分分析中的应用

离子色谱是用于分离分析不同基质样品中离子性物质的一种新型高效液相色谱技术。自1975年发展至今,已被广泛应用于环境、能源、食品、医药等多个领域,具有操作简单、分析快速、灵敏度和选择性高,且能同时分离测定多种组分等优点。近年来,随着离子色谱技术自身迭代发展,可测定分析的样品种类已包括离子、糖类、氨基酸、有机酸(碱)等,同时离子色谱法也越来越成为针对中草药复杂组分中单个有效成分分析与鉴定的重要手段。本文介绍了离子色谱技术的不同类型、原理及研究进展,整理了近几十年离子色谱在中草药糖苷类、氨基酸、蛋白质、无机盐以及有机酸、生物碱类和黄酮类等复杂成分中的应用情况;检索文献发现,离子交换色谱、电导检测法为离子色谱中最常用的技术类型和检测方式,且目前离子色谱在生物碱类成分分析中的应用展现出较传统分析方法更好的优势,但在无机阴离子的形态分析和黄酮类、苯丙素类、甾体类等主要活性物质中的直接应用研究报道较少。最后,综述了离子色谱(联用)新技术及其在中草药中的最新进展,并对该色谱方法未来在复杂组分分离分析方面的应用进行了探讨和展望,为离子色谱技术分析中草药复杂化学成分的进一步发展提供理论参考。     

毛细管电泳技术在药物分离分析中的研究与应用

综述了近5年毛细管电泳在手性药物拆分、药物制剂及中草药分析中的应用.在手性药物拆分的应用中主要探讨了手性选择剂的种类及毛细管分离方法;在药物制剂、中草药的应用中主要介绍该法对药效成分进行的分离及定量分析,总结方法的检出限、线性范围和检测方法;最后,探讨了毛细管电泳在求取药物水解常数上的应用.提出毛细管电泳在药物分析中将有广阔的应用前景.     

温敏水凝胶溶胀行为及其分离性能

以甲基丙烯酸钠(SM)为单体与异丙基丙烯酰胺(NPA)共聚,N,N-亚甲基双丙烯酰胺(MBA)为交联剂,得到阴离子型温敏水凝胶;对其热敏性能、溶胀性能及它对甘草酸的分离性能进行了研究,并通过凝胶中水的状态理论对结果进行了分析和解释,还研究了阴离子浓度的变化对上述性能的影响。将其用于甘草酸粗品的分离吸收,探讨它用于分离中草药有效成分的可能性。     

自动进样分光光度法测定中草药中的铈

<正>稀土是植物生长发育的有益元素[1-4]。我国中草药应用已有几千年的历史,稀土和微量元素对中草药药效的影响以及稀土元素在中草药方面的应用是药学科学研究的新领域。将稀土元素用于中草药,可提高中草药产量与质量,并提高中草药有效成分含量,最终可提高药物疗效[5-8],因此,检测中草药中稀土元素的含量有着十分重要的意义。稀土元素与偶氮胂Ⅲ在弱酸性环境中显色反应十分灵敏,据此,可用紫外-可见分光光度法直接测     

现代电化学分析技术在中药研究领域中的应用与前景

本文综述了近年来各种现代电化学分析技术在中草药分析领域的研究现状与进展, 引用文献177 篇。通过对合成药物和天然药物研究状况的对比, 着重介绍了中草药有效成分和微量元素分析中各种现代电化学分析技术的应用。     

高效液相色谱指纹图谱在中药芦根上的应用

利用现代分离分析技术如高效液相色谱(HPLC)与气相色谱(GC),能够获得中草药的色谱指纹图谱。本实验报道了高效液相指纹图谱应用于快速检测中草药提取物以及应用于研究、开发与生产中的质量控制体系中,利用HPLC建立芦根的色谱指纹图谱。实验条件为反相C18柱,流速为1．0mL／min,紫外检测器(λ=230nm)。通过分析比较色谱指纹图谱中的相对保留值α以及相对面积St对不同产地的芦根进行对比研究。这种基于HPLC的分析策略为中草药的精确鉴定和质量控制提供了有效的信息,并为HPLC在复杂组分样品中的应用开拓了新的领域。     

中药有效成分三维结构数据库的开发和研究

介绍了北京大学中药有效成分三维结构数据库软件系统的结构、功能及开发步骤。该数据库系统不仅仅提供6500个中草药有效成分的二维和三维结构以及其它各类相关信息,同时拥有功能强大的数据库查询、维护及分子表达系统。在该系统中,用户可以交互式地实现多种分子特征的查询以及二维子结构的查询。查询得到的分子可以直接在北京大学药物设计系统(PKUDDS)中进行三维结构的显示和分析。该数据库系统和我们科研组开发的北京大学药物设计系统以及中草药信息系统构成了完整的基于中药的药物设计系统。该系统已经用于NS3-NS4A蛋白酶抑制剂以及其它体系的研究并取得了很好的结果。     

Capillary electrophoresis with amperometric detection of curcumin in Chinese herbal medicine pretreated by solid-phase extraction

In the present study, curcumin from Chinese herbal medicine turmeric was determined by capillary electrophoresis with amperometric detection (CE-AD) pretreated by a self-designed, simple, inexpensive solid-phase extraction (SPE) cartridge based on the material of tributyl phosphate resin. An average concentration factor of 9 with the recovery of > 80% was achieved when applied to the analysis of curcumin in extracts of tumeric. Under the optimized CE-AD conditions: a running buffer composed of 15 mM phosphate buffer at a pH 9.7, separation voltage at 16 kV, injection for 6 s at 9 kV and detection at 1.20 V, CE-AD with SPE exhibited low detection limit as 3 x 10(-8) mol/l (S/N = 3), high efficiency of 1.0 x 10(5) N, linear range of 7 x 10(-4) -3 x 10(-6) mol/l (r = 0.9986) for curcumin extracted from light petroleum. The method developed resulted in enhancement of the detection sensitivity and reduction of interference from sample matrix in complicated samples and exhibited the potential application for routine analysis, especially in food, because a relatively complete process of sample treatment and analysis was described.     

玄参、生地黄、紫草等六种中药中微量元素含量的测定

为了解中药中微量元素的含量与其药物的作用机制关系,用原子吸收分光光度计测定了玄参、生地黄、紫草、水牛角、牡丹皮、赤芍中铁(Fe)、镁(Mg)、铜(Cu)、钙(Ca)、锌(Zn)、铬(Cr)、钼(Mo)等7种微量元素的含量.结果表明,Ca的含量最高,Cu的含量几乎最低.这6种中草药含有多种对人体有益的微量元素,与它们的药...     

Phytochemical analysis of traditional Chinese medicine using liquid chromatography coupled with mass spectrometry

Traditional Chinese medicine (TCM) is commonly considered to operate due to the synergistic effects of all the major and minor components in the medicines. Hence sensitive and comprehensive analytical techniques are needed to acquire a better understanding of the pharmacological basis of the herb and to enhance the product quality control. The present review mainly focuses on the phytochemical analysis of TCMs using high-performance liquid chromatography coupled with mass spectrometry (HPLC-MS). Atmospheric pressure chemical ionization (APCI) and electrospray ionization (ESI) are the two commonly used ion sources. Triple quadrupole, ion trap (IT), Fourier transform ion cyclotron resonance (FTICR) and time-of-flight (TOF) mass spectrometers are used as on-line analyzer. The relationship between structural features and fragmentation patterns should be investigated as thoroughly as possible and hence be applied in the on-line analysis to deduce the structures of detected peaks. Characteristic fragmentation behaviors of the reference standards, as well as information regarding polarity obtained from retention time data, on-line UV spectra, data from the literature and bio-sources of the compounds allowed the identification of the phytochemical constituents in the crude extracts. Although a mass spectrometer is not a universal detector, high-performance liquid chromatography coupled with multistage mass spectrometry (HPLC-MS(n)) technique was still proved to be a rapid and sensitive method to analyze the majority of the many constituents in herbal medicines, particularly for the detection of those present in minor or trace amounts. The methods established using HPLC-MS techniques facilitate the convenient and rapid quality control of traditional medicines and their pharmaceutical preparations. However, the quantitative analysis is not the topic of this review.     

18种中药中微量元素铁锌锰铜的含量研究

为研究治疗黄褐斑常用中药中Fe、Zn、Cu、Mn的含量与药效的关系,测定了18种中药材中Fe、Zn、Cu、Mn含量,并用主成分分析法进行分析.结果表明,Fe含量最高,Zn、Mn次之,Cu最少;Zn和Cu的相关系数最大,且Zn与Cu比均大于1.说明补充Zn可以抑制Cu与酶结合,防治色斑.     

Chemical fingerprinting of Gardenia jasminoides fruit using direct sample introduction and gas chromatography with mass spectrometry detection

A rapid, rugged, and inexpensive approach is described to develop chemical fingerprints of volatile and semivolatile fractions in herbal medicine. The method is based on the combination of direct sample introduction and gas chromatography (GC) analysis with mass spectrometry detection. In comparison with routine methods, the proposed approach provides the most informative fingerprint and does not demand time-consuming extraction, pretreatment, and cleanup procedures. The approach was applied to establish the GC fingerprint of gardenia fruit (Gardenia jasminoides Ellis), in which 39 components were identified. With the help of principal components analysis, the obtained fingerprint could reveal the variation in and within different herb samples as affected by season and developmental state (wild or cultivated). The results indicated that the proposed approach could serve as a rapid, simple, and effective technique for the quality control of herbal medicines.     

A novel capillary electrophoretic method for determining aliphatic aldehydes in food samples using 2-thiobarbituric acid derivatization

A novel electrophoretic method for sensitive determination of nine aldehydes, including formaldehyde (C1), acetaldehyde (C2), propanal (C3), butanal (C4), pentanal (C5), hexanal (C6), glutaradehyde (Gla), 2,3-butanedione (Bud) and methylgloxal (MGo) in food samples, has been developed based on CE with amperometric detection (CE-AD). After being derivatized with an electroactive compound, 2-thiobarbituric acid (TBA), these nine non-electroactive aldehydes were converted to electroactive adducts, and therefore detectable by CE-AD approach. Experimental conditions of derivatization and CE-AD detection were optimized. The proposed method was validated according to International Conference on Harmonization (ICH) requirements, with recovery results ranging from 82.8 to 123.8%. Calibration plots of aliphatic aldehydes were linear (r2 ≥ 0.9901) in the concentration range from 0.083 to 15.0 mg/L. The LODs were between 0.008 and 0.074 mg/L. The proposed CE-AD method provides a reliable and sensitive quantitative evaluation for non-electroactive low-molecular-mass monoaldehydes and dialdehydes in real sample matrices by employing relatively simple and inexpensive instrument.     

薏苡仁中黄曲霉毒素G1的动态表面增强拉曼光谱检测

中药具有不良反应少,疗效独特等优点,越来越受到国内外的关注。但中药在生产、采集、加工、运输、贮藏等方面极易发生霉变而污染黄曲霉毒素。黄曲霉毒素具有很强的毒性,不仅影响中药质量和疗效还会对人体肝脏等器官造成极大损害。该文建立了中药材薏苡仁中黄曲霉毒素G1(Aflatoxin G1,AFG1)的动态表面增强拉曼光谱(Dynamic Surface-enhanced Raman Spectroscopy,D-SERS)的快速分析方法。采用简单擦拭法提取薏苡仁表面的黄曲霉毒素G1,因此SERS图谱中干扰峰较少。并且以金纳米颗粒为增强基底,优化了检测条件,进行了黄曲霉毒素G1的D-SERS的检测与分析。结果表明,方法的线性范围为8~320μg/kg,线性方程为y=0.0293x+1.7307,相关系数(r2)为0.9884。检出限(LOD)为5.5μg/kg,相对标准偏差(RSD)为11%。该方法的线性良好,灵敏度和重现性均能满足薏苡仁中黄曲霉毒素G1的快速检测要求,且操作简单、快速、节约成本,对中药材中黄曲霉毒素G1的现场实时快速分析具有良好的应用潜力。     

Determination of Pesticides in the Rhizome of Traditional Chinese Medicines by Gas Chromatography with Electron Capture Detection

A simple and efficient gas chromatography method for the determination of 27 organochlorine and pyrethroid pesticides in traditional Chinese medicine was developed. Pesticide residues were extracted from the samples by oscillation and ultrasound, and purified by gel permeation chromatography and florisil solid phase extraction. The analysis was performed by gas chromatography with micro-electron capture detection. The purification conditions, such as the extraction and elution solvents, extraction methodology, and gel permeation chromatography conditions, were optimized. Traditional Chinese medicines were purified by different methods based on their composition. Under optimized conditions, the calibration graph was linear from 10 to 500 µg/L and the correlation coefficients varied from 0.9958 to 0.9997. The detection limits of these pesticides were between 0.09 and 1.82 µg/kg. The recovery of the pesticides spiked in various samples at four concentrations ranged from 73.2% to 106.4%, with relative standard deviations between 1.0% and 14.0%. This study indicates that the method is useful for determining pesticides in rhizome traditional Chinese medicines.     

汽爆技术促进中药资源高值化利用

汽爆技术在中药资源高值化利用中发挥的作用正在逐渐体现:汽爆处理打破中药植物细胞壁的屏障结构,有利于有效成分的分离提取;汽爆过程物料自体水解发生去糖苷化作用使天然植物中的苷元与糖基分离,提高苷类物质提取和分离效率;汽爆应用于中药炮制和中药脱毒有高效、快速和避免有效成分流失等优点;汽爆处理有利于中药非药用组分如纤维素、半纤维素等的有效分离和利用,联产乙醇、丁醇等能源和化工产品。本文对汽爆技术在中药资源高值化利用中的研究进展进行了综述。