Study on Gas Chromatographic Separation and Analysis Theory for Unknown Complex Samples

复杂未知样品的分离与分析是目前分析化学的热点和难点之一。气相色谱是用于挥发性物质分析的最常用工具，是与质谱、红外等联用的基本分离手段。本论文针对复杂未知样品的气相色谱分离与分析，开展了程升条件下保留值及峰形规律的研究，发展了快速获取气相色谱保留参数、峰形参数及峰形规律、优化分析条件的方法及软件系统，提高了气相色谱分析方法发展的效率和可靠性及定性定量的精确性。发展了利用Levenberg-Marquardt法从几次程序升温条件快速获取气相色谱保留参数(A, B参数)及基于内标化合物对预测保留时间的精确校正方法。研究认为等起点的辐射状程升模式是获取A, B参数的理想预实验模式；计算A, B参数时应包含至少3个升温速率差别较大的程升条件。由单柱程升A, B参数和双柱换算A, B参数得到的校正保留时间的平均误差分别小于2秒和5秒

一种精确测定色谱峰形参数和重叠峰面积的方法

一种精确测定色谱峰形参数和重叠峰面积的方法，其特征在于：(1) 给定待测定色谱流出曲线(tk，hk)和峰数目q，tk，hk分别为流出曲线段中k点的时间值和色谱信号值，k＝1，2，…，n，n为总点数；(2)以高斯模型或指数修正的高斯模型为目标函数，对上述待测定色谱流出曲线进行峰拟合，通过非线性最小二乘法求出目标函数即拟合流出曲线的最佳参数，进而根据拟合流出曲线与待测定色谱流出曲线的对应关系，对应出待测定色谱峰形参数和重叠峰面积。本发明能快速、准确、方便地测量色谱峰形参数和重叠峰面积。带填

组分中药色谱分离方法学研究

Presently, Traditional Chinese Medicine (TCM) is an important resource to treat many diseases, which has a long history in China, and is very complicated in chemical composition and pharmacology. Therefore, modernization of TCM is very necessary, including standardization, resourcing, quality control and research on chemical composition and pharmacology. “Multi-Component Chinese Medicine (MCCM)” represents a specific group of chemical composition produced from TCM according to a standardized separation process, which is hopefully to discover the chemical fundament of TCM’s pharmacology. The systematic research on MCCM is basing on modern separation and analytical techniques. In our group, a high-throughput preparation method has been developed in order to accelerate the pharmacological study of MCCM. The whole of TCMs were separated into a serious of small fractions containing several compounds by high-throughput preparative chromatography. Then these small fractions, what is called screening multi-components (SMCs), were screened by high-throughput screening (HTS). After biological screening, active multi-components were obtained and could be studied deeply further. This method will accelerate the process of explanation of the curative mechanism of TCMs, which simplifies the complex TCMs by concentrating on those interesting compounds from hundreds of thousands of compounds in TCMs. Standard libraries of SMCs are constructed, which will not only satisfy the need of TCMs, but also will speed up drug discovery by supplying persistent source for HTS. Two-dimensional liquid chromatography (2DLC) systems have developed for the characterization of SMCs and preparation of active compounds. Orthogonality and compatibility between the two-dimensional separations are key factors affecting the development of 2DLC. Based on the development of novel stationary phases, RP-HILIC 2DLC system and RP-RP 2DLC system were established.Two-dimensional liquid chromatography (2DLC) systems have developed for the characterization of SMCs and preparation of active compounds. Orthogonality and compatibility between the two-dimensional separations are key factors affecting the development of 2DLC. Based on the development of novel stationary phases, RP-HILIC 2DLC system and RP-RP 2DLC system were established

复杂样品分离分析方法学

Traditional Chinese Medicine (TCM) is a typical complex sample. Our data showed that there were at least ten thousands of compounds in one kind of TCM. These compounds are very different in their structures, polarity, content, etc. Therefore, the separation and analysis of TCM is a huge challenge for scientists. The systematic research on TCM is carrying out from different levels such as high polar components, homologue components and minor components in our lab. The study on separation of high polar compounds in TCM needs to be strengthened. Hydrophilic interaction chromatography (HILIC) has a great potential for separation and analysis of high polar compounds in TCM. High-throughput preparation and highly orthogonal separation is the main strategy to obtain pure compounds from TCM. Complex extracts are separated to a large number of fractions using high-throughput preparation. Most of fractions contain several compounds but some are still complex. Highly orthogonal separation is quite essential in isolation of high-purity compounds from these complex fractions and purity assessment of those pure compounds. Development of novel separation materials is the key point of resolve the problem in separation of TCM. The separation of high polar compounds needs to develop novel HILIC stationary phases. The development of orthogonal stationary phases is of significant importance in highly orthogonal separation. In general, the development of methodology for separation and analysis of TCM from different levels is on the base of development of novel separation material in various separation modes and under the guidance of the strategy of high-throughput preparation and highly orthogonal separation