液相色谱-串联质谱法在药物代谢研究中应用最新进展

液相色谱-质谱联用技术因其具有高分离能力、高灵敏度、应用范围广和较强的专属性等特点,已成为一种重要的现代分离分析技术。串联质谱法比单极质谱具有更高的灵敏度和选择性,可以得到更多的结构信息。本文首先介绍了液相色谱-串联质谱法中串联质谱基本原理、常见质谱质量分析器及其特点、串联质谱的连接方式和数据采集方法等。然后将其在药物代谢研究中的主要应用作简要介绍,主要包括利用串联质谱测定药物的代谢动力学参数,利用几种串联质谱应用方式对药物代谢物的结构进行鉴定,概括了每种方式的优劣,总结了串联质谱在药物代谢物结构鉴定中的应用策略,并对其在药物代谢未来的应用进行了展望。     

大鼠胆汁中β-榄香烯代谢产物的研究

目的　研究大鼠胆汁中β-榄香烯的代谢产物。方法　采用质谱、核磁共振、红外、紫外分析法对iv β-榄香烯后大鼠胆汁样品进行分析。结果　确定了一个代谢产物的结构为1-甲基-1-乙烯基-2-异丙烯基-4-异丙烯醛基环己烷。结论　β-榄香烯在体内存在生物转化过程。     

Mass spectrometric analysis of anatoxin-a

Secondary ion mass spectrometry (SIMS), gas chromatography/mass spectrometry (GC/MS), desorption chemical ionization/mass spectrometry (DCI/MS), and thermospray/mass spectrometry (TSP/MS) were evaluated for the detection of a low-molecular weight biological toxin, anatoxin-a. The lowest detection limit was obtained using isobutane or ammonia DCI/MS. Tandem mass spectrometry (MS/MS) was used to enhance the selectivity and sensitivity of the analysis. The detection limit for the pure material is 10 pg, and 100 pg of the toxin can be analyzed directly from urine using DCI/MS/MS.     

Plasma desorption mass spectrometry of large biomolecules

Two mass spectrometric techniques, plasma desorption mass spectrometry (PDMS) and fast atom bombardment mass spectrometry (FABMS), are now extensively used for characterisation of large biomolecules. Mass spectra of protein molecules up to 34 kDa have been observed and mass spectrometry has been demonstrated to be an effective analytical tool for protein chemistry and biotechnology. Also carbohydrates and oligonucleotides can be analysed by mass spectrometry, but further improvements of the techniques are needed.     

生物质谱技术的发展及在蛋白质结构研究中的应用

综述生物质谱技术的发展现状，包括电喷雾电离质谱、基质辅助激光解吸电离质谱、串联质谱、电喷雾解吸电离质谱、表面增强激光解吸电离-飞行时间质谱等，以及这些技术在蛋白质结构研究中的应用进展。生物质谱技术已成为蛋白质结构研究的重要工具。     

Analysis and screening of combinatorial libraries using mass spectrometry

Mass spectrometry is a highly selective and high throughput analytical technique that is ideally suited for the identification and purity determination of large numbers of compounds prepared using combinatorial chemistry or for the dereplication of natural products. Compounds may be characterized based on molecular weight, elemental composition and structural features based on fragmentation patterns. When coupled to a separation technique such as high-performance liquid chromatography (HPLC) or capillary electrophoresis, mass spectrometric applications may be expanded to include analysis of complex mixtures. However, the slower speed of the separation step reduces the throughput of the analysis. This review concerns the application of mass spectrometry to the characterization of combinatorial libraries and the screening of library and natural product mixtures. Strategies to enhance the throughput of LC-MS are discussed including fast HPLC and parallel LC-MS. Also, mass spectrometry-based screening methods are described including frontal affinity chromatography-mass spectrometry, gel permeation chromatography LC-MS, direct electrospray mass spectrometry of receptor-ligand complexes, affinity chromatography-mass spectrometry, and pulsed ultrafiltration mass spectrometry.     

九种药用真菌中微量元素的含量

作者用原子吸收分光光度法和等离子体发射光谱法测定了九种药用真菌中十四种微量元素的含量。     

Comparison of different serum sample extraction methods and their suitability for mass spectrometry analysis

Mass spectrometry has been widely used, particularly in pharmacokinetic investigations and for therapeutic drug monitoring purposes. Like any other analytical method some difficulties exist in employing mass spectrometry, mainly when it is used to test biological samples, such as to detect drug candidates in mammalian serum, which is rich in proteins, lipids and other contents that may interfere with the investigational drug. The complexity of the serum proteome presents challenges for efficient sample preparation and adequate sensitivity for mass spectrometry analysis of drugs. Enrichment procedures prior to the drug analysis are often needed and as a result, the study of serum or plasma components usually demands either methods of purification or depletion of one or more. Selection of the best combination of sample introduction method is a crucial determinant of the sensitivity and accuracy of mass spectrometry. The aim of this study was to determine the highest serum protein precipitation activity of five commonly used sample preparation methods and test their suitability for mass spectrometry. We spiked three small molecules into rabbit serum and applied different protein precipitation methods to determine their precipitation activity and applicability as a mass spectrometry introductory tool.