高效液相色谱-核磁共振仪联用技术在耐哌地尔杂质检测中的应用

用高效液相色谱-核磁共振（HPLC-CNM）联用技术中的连续流动和停止流动两种模式对萘哌地尔中杂质进行检测,根据^1HNMR,^1H-^1HCOSY谱完成了主要杂质1-萘环-丙三醇结构鉴定。HPLC-NMR是解决合成药物中杂质结构确证的简便、快速方法。     

食用油甘油三酯质谱分析方法的研究进展

该文对质谱鉴定技术及其与色谱联用的分析方法(包括直接进样质谱分析、气相色谱质谱联用技术、超临界流体与质谱联用技术和液相色谱质谱联用技术)在甘油三酯分析方面的应用进行了综述,评述了各类分析方法的优缺点,对常用的脂质分析数据库进行了介绍,并对甘油三酯分析方法的发展及应用作了展望。     

Advances 0n Analysis of Triacylglycerols in Edible Oil Based on Mass Spectrometric Method

该文对质谱鉴定技术及其与色谱联用的分析方法(包括直接进样质谱分析、气相色谱质谱联用技术、超临界流体与质谱联用技术和液相色谱质谱联用技术)在甘油三酯分析方面的应用进行了综述,评述了各类分析方法的优缺点,对常用的脂质分析数据库进行了介绍,并对甘油三酯分析方法的发展及应用作了展望.     

联用技术在生物体系化合物分析中的应用进展

介绍了目前分离分析生物体系化合物的一般步骤和注意事项.综述了联用技术在生物体系化合物分析中的应用进展情况.展望了联用技术在生物体系化合物分析中的发展方向和应用前景.     

热分析联用技术及其在金属材料领域中的应用

热分析联用技术是在热重分析基础上,将多种检测手段并用,准确地研究材料的结构、组成、热反应等特性,从而揭示材料热分解过程本质的技术。在程序升温过程中,利用热分析联用技术对金属材料的质量和热量变化及热分解产物成分等信息进行检测,能更精准地研究金属材料的组成和热分解特性。该文在热重分析法的基础上,着重介绍了其与差热分析、差示扫描量热分析、傅里叶红外光谱分析、质谱分析等分析方法的联用,并以金属材料研究为例,分析了热分析联用技术在金属材料的结构、性能测定等方面的应用,同时展望了热分析联用技术的应用前景。     

质谱分析技术在纺织品检测方面的应用

介绍纺织品中有害物质标准检测方法中质谱分析技术的应用,概述了气相色谱-质谱联用、高效液相色谱-质谱联用和电感耦合等离子体-质谱联用技术在纺织品检测方面的广泛应用及其发展前景.     

电感耦合等离子体质谱(ICP-MS)联用技术的应用及展望

总结了ICP-MS联用技术在国内外检测领域的最新应用,并就"分离器与ICP-MS"、"进样系统与ICP-MS"、"ICP-MS与其它仪器物理联用"等联用技术进行了分类、拓展和总结。ICP-MS联用技术的发展重点将倾向于提高分析精密度、复杂基体元素超痕量分析、同位素比值及形态研究领域,相关联用技术的国家标准或行业标准出台已迫在眉睫。     

固相表面荧光光谱法在药物分析中的应用

本文综述了近十年来固相表面荧光光谱法、固相萃取-固相表面荧光联用技术以及流动注射分析、顺序注射分析和可更新表面技术与固相表面荧光联用技术在药物分析中的应用.展望了固相表面荧光光谱法在药物分析中的发展趋势和前景.     

高效液相色谱-电感耦合等离子体质谱联用技术在水质分析中的应用

对高效液相色谱-电感耦合等离子体质谱联用技术在水质分析中的应用作了评述,对高效液相色谱-电感耦合等离子体质谱联用技术的发展前景作了展望.引用文献48篇.     

二维气相色谱技术及其在烟草行业中的应用

二维气相色谱的应用大大提高了分析能力,而与飞行时间质谱的联用更使其达到一个新的高度。介绍了二维气相色谱的原理、优越性及不足,以及与飞行时间质谱联用的技术进展。综述了近年来该技术在各行业特别在烟草行业中的应用,展望了二维气相色谱在烟草行业中的应用前景。     

高效液相色谱-核磁共振联用技术最新进展

介绍了ＨＰＬＣ－ＮＭＲ技术的最新发展状况,讨论了ＨＰＬＣ－ＮＭＲ技术在应用中面临的问题和解决方法,评述了ＨＰＬＣ－ＮＭＲ两种主要操作方式：连续流和驻流方式,并介绍了ＨＰＬＣ－ＮＭＲ技术的应用情况,最后对其今后的发展方向作了预测。     

HPLC-NMR of fatty alcohol ethoxylates

The application of HPLC-NMR for the analysis of a mixture of fatty alcohol ethoxylates (FAEs) is described. The use of the new generation, cryogenically cooled probes is investigated in respect of the sensitivity advantage that they provide. The FAE mixture is separated using liquid chromatography at the critical point of adsorption. The ability of the method to differentiate between the different end groups and the degree of polymerization of the mixture constituents is investigated. Both on-flow and stop-flow HPLC-NMR techniques were used together with two-dimensional NMR spectroscopy. The results are compared with those obtained by using an evaporative light scattering detector for the HPLC.     

Application of HPLC-NMR coupling using C30 phase in the separation and identification of flavonoids of taxonomic relevance

The on-line separation and identification of two important taxonomic markers for plant species of the Paepalanthus genus, the flavonoids 6-methoxykaempferol-3-O-beta-D-glucopyranoside and 6-methoxykaempferol-3-O-beta-D-6"(p-coumaroyl)glucopyranoside, has been performed with an HPLC-NMR coupling using C30 phase. 1D spectra have been recorded in the stopped-flow mode for the two predominant chromatographic peaks. This is the first application of HPLC-NMR coupling using C30 phase to a taxonomic problem. The technique drastically reduces the required amount of sampling for structure determination.     

Implementation of real-time two-dimensional nuclear magnetic resonance spectroscopy for on-flow high-performance liquid chromatography

Directly coupled HPLC-NMR has become a powerful tool for separation and structural elucidation of unknown compounds. However, there are only a few reports on application of on-flow two-dimensional (2D) NMR in HPLC-NMR. Here we present an alternative method for recording real-time 2D-NMR spectrum (total correlation spectroscopy, TOCSY) on a commercial HPLC-NMR system. The method is based on well-established Hadamard matrix for 2D-NMR frequency encoding. In addition, a modified/improved solvent suppression approach is incorporated. This makes it possible to carry out the experiment with both polar and gradient eluents, the widely used chromatographic conditions. The method is example using a synthesized mixture of three amino acids (His, Phe and Try) and a human urine sample. The method demonstrated here may be utilized for high-throughput structural or unknown component identification and fast dynamic study in a variety of applications.     

Real-time separation of natural products by ultrafast 2D NMR coupled to on-line HPLC

Hyphenated HPLC-NMR is an extremely efficient analytical tool, which makes it possible to perform on-flow experiments where 1D NMR spectra are obtained in real time as the analytes are separated and eluted from the chromatographic column. However, it is incompatible with multidimensional NMR methods that form an indispensible tool for the study of complex mixtures. Recently, Frydman and co-workers have proposed an ultrafast 2D NMR approach, where a complete 2D NMR correlation can be recorded in a single scan, thus providing a solution to the irreversibility of hyphenated techniques. This paper presents the first implementation of on-line ultrafast HPLC-NMR. Ultrafast COSY spectra are acquired every 12 s in the course of a chromatographic run performed on a mixture of natural aromatic compounds. The results, obtained on a commercial HPLC-NMR setup, highlight the generality of the ultrafast HPLC-NMR methodology, thus opening the way to a number of applications in the numerous fields in which HPLC-NMR forms a routine analytical tool.     

Application of HPLC-NMR coupling using C30 phase in the separation and identification of flavonoids of taxonomic relevance

The on-line separation and identification of two important taxonomic markers for plant species of the Paepalanthus genus, the flavonoids 6-methoxykaempferol-3-O-β-D-glucopyranoside and 6-methoxykaempferol-3-O-β-D-6″(p-coumaroyl)glucopyranoside, has been performed with an HPLC-NMR coupling using C₃₀ phase. 1D spectra have been recorded in the stopped-flow mode for the two predominant chromatographic peaks. This is the first application of HPLC-NMR coupling using C₃₀ phase to a taxonomic problem. The technique drastically reduces the required amount of sampling for structure determination. Received: 20 March 2000 / Revised: 14 June 2000 / /Accepted: 23 June 2000     

High performance liquid chromatography coupled to nuclear magnetic resonance spectroscopy and mass spectrometry applied to plant products: Identification of ecdysteroids fromSilene otites

Summary HPLC coupled in parallel to nuclear magnetic resonance (NMR) and mass spectrometry (MS) has been used to obtain¹H NMR and mass spectra of a number of ecdysteroids present in an extract of the plantSilene otites. Reversed phase gradient chromatography was performed using a D₂0-acetonitrile-based solvent system. NMR and mass spectra were obtained for integristerone A, 20-hydroxyecdysone, 2-deoxy-20-hydroxyecdysone and 2-deoxyecdysone to provide structural confirmation using continuous and stopped flow HPLC-NMR. The combined HPLC-NMR-MS system described here provided a more comprehensive analysis of the ecdysteroids present in the extract than HPLC-NMR alone.     

Hyphenated HPLC-NMR and its applications in drug discovery

Hyphenated HPLC-NMR is a fast growing technology, allowing rapid and detailed structural characterization of unknown mixtures. The technical aspects of the technology are reviewed on the basis of system configuration, operation, solvent suppression, HPLC and NMR optimization, and detection. The combined use of HPLC-NMR and HPLC-MS is also described and discussed. Various applications of HPLC-NMR and integrated HPLC-NMR-MS in drug discovery, especially in the separation and structure elucidation of drug impurities, reaction mixtures, degradation products, in vitro and in vivo metabolites, and combinatorial library samples, are illustrated.     

Anwendungsbeispiele der direkten HPLC-NMR-Kopplung mit hoher Aufl?sung

Zusammenfassung Durch HPLC-NMR on-line Kopplung ist eine gleichzeitige Trennung und Identifizierung von Komponenten eines Substanzgemisches möglich. Trennbeispiele von Aromaten und Steroiden zeigen die mögliche Anwendungsbreite der Methode durch Messung im Durchfluß-bzw. stop-flow-Verfahren. Durch Verwendung einer mathematischen Filter-Funktion kann annähernd die Qualität von herkömmlichen Routine-Spektren erzielt werden.

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Examples of application of direct HPLC-NMR-coupling with high resolution

Summary With the direct on-line coupling of HPLC-NMR, simultaneous separation and identification in the liquid phase of components in a mixture is possible. Examples carried out on some aromatic compounds as well as steroids show the wide scope of application of this method with either a continuous flow or a stop flow technique. A mathematical resolution enhancement technique is utilized to improve the on-line NMR spectra substantially.

     

Multiple hyphenation of liquid chromatography with nuclear magnetic resonance spectroscopy, mass spectrometry and beyond

The advent of sensitive and reliable HPLC-NMR and HPLC-MS systems has revolutionised the identification of compounds eluting from chromatographic systems. More recently systems have been described wherein both NMR and MS are used together to provide an immensely powerful means of characterising compounds in chromatographic eluents. Here the construction and application of combined HPLC-NMR-MS systems to the analysis of mixtures of pharmaceuticals, drug metabolites in biological fluids and natural products in plant extracts is reviewed. In addition preliminary work with alternative systems such as HPLC-UV-NMR-FTIR-MS is highlighted and the prospects for such complex systems considered.