分子生物色谱用于中药活性成分筛选及质量控制方法的研究

报道了近期工作进展,首先阐述了分子生物色谱的基本原理及特点,然后介绍了分子生物色谱对多种中药、不同产地的同种中药活性成分谱图模式的比较,结合已有的工作对活性成分筛选方法、相互作用研究、质量控制方法发展做了细致的说明,并讨论了其发展方向及前景。     

基于MATLAB开发的核磁共振波谱信息库

基于核磁共振原理及NMR谱图的解析和检索方法,利用MATLAB语言的开放式可扩充式体系结构特点,介绍了核磁共振波谱图谱信息库的特点、设计方法、技术处理及系统应用。     

《色谱定性与定量》(第二版)

该书主要介绍了色谱分析中常用的定性和定量方法。在定性分析中除了介绍经典的保留值定性的各种方法外,对近年来在色谱定性分析中使用的质谱和红外光谱的谱图解析作了较详细的介绍。定量分析中除了介绍各种定量分析方法外,对数据处理中的误差分析、定量结果的评价和表达方法作了详细介绍。     

无机化学综合实验:葡萄糖酸锌的制备与成分分析

介绍了一个集无机化学、分析化学、仪器分析于一体的无机化学综合实验。通过不同方法制备得到葡萄糖酸锌,并对其成分进行分析,使学生掌握蒸发、浓缩、过滤、结晶等基本操作,学习配位滴定的原理及操作,了解红外光谱检测法及谱图解析。采用分组形式以不同方法制备产物,并对实验结果进行探讨和拓展。学生比较了不同制备方法的优劣,解决了实验过程中的存疑,锻炼和提高了综合实验能力。     

《色谱定性与定量》（第二版）

该书主要介绍了色谱分析中常用的定性和定量方法。在定性分析中除了介绍经典的保留值定性的各种方法外,对近年来在色谱定性分析中使用的质谱和红外光谱的谱图解析作了较详细的介绍。定量分析中除了介绍各种定量分析方法外,对数据处理中的误差分析、定量结果的评价和表达方法作了详细介绍。     

《色谱定性与定量》（第二版）

该书主要介绍了色谱分析中常用的定性和定量方法。在定性分析中除了介绍经典的保留值定性的各种方法外,对近年来在色谱定性分析中使用的质谱和红外光谱的谱图解析作了较详细的介绍。定量分析中除了介绍各种定量分析方法外,对数据处理中的误差分析、定量结果的评价和表达方法作了详细介绍。     

《色谱定性与定量》(第二版)

该书主要介绍了色谱分析中常用的定性和定量方法。在定性分析中除了介绍经典的保留值定性的各种方法外,对近年来在色谱定性分析中使用的质谱和红外光谱的谱图解析作了较详细的介绍。定量分析中除了介绍各种定量分析方     

振动圆二色谱: 一种确定手性分子绝对构型的新方法

手性分子绝对构型的确定是一个极其重要且长期存在的问题. 振动圆二色谱是在红外波长区域测定分子圆二色性的一种新方法, 极大地扩展了圆二色谱的应用范围. 振动圆二色谱法通过构象搜索、量子化学计算等手段准确预测手性分子的振动圆二色谱图, 进而与实测谱图进行比较确定其绝对构型. 该方法已经得到了越来越广泛的应用, 必将成为一种有效测定手性分子绝对构型的常规方法.     

XPS中Tougaard法本底扣除初探

介绍了XPS（X ray photoelectron spectroscopy）谱图中本底产生的机理以及Tougaard法本底扣除原理的简略推导过程,提出了可供编程的约化形式,使用VC语言编写程序试对不同样品（含金属、过渡金属及非金属）的谱图进行本底扣除,并与Shirley法、直线法本底扣除进行准确性的比较,提出了Tougaard方法试用于非金属粉末化合物样品的测试分析结果.     

XPS中Tougaard法本底扣除初探

介绍了XPS(X-ray photoelectron spectroscopy)谱图中本底产生的机理以及Tougaard法本底扣除原理的简略推导过程,提出了可供编程的约化形式,使用VC语言编写程序试对不同样品(含金属、过渡金属及非金属)的谱图进行本底扣除,并与Shirley法、直线法本底扣除进行准确性的比较,提出了Tougaard方法试用于非金属粉末化合物样品的测试分析结果.     

二维相关振动光谱技术

从发展历史、计算方程、性质规则等方面系统地介绍了近年来发展起来的二维相关光谱技术.结合各种常见的一维振动光谱, 如红外、拉曼、荧光、近红外-红外等光谱举例阐述了二维振动光谱的优势及其普适性.介绍了在广义二维相关光谱理论上最新延伸发展起来的二维样品-样品相关技术和二维杂化相关技术的基本理论, 并将之与传统的二维变量-变量相关技术(广义二维相关光谱)进行了比较.     

Recent developments in two-dimensional (2D) correlation spectroscopy

Recent noteworthy developments in the field of two-dimensional(2D) correlation spectroscopy are reviewed.2D correlation spectroscopy has become a very popular tool due to its versatility and relative ease of use.The technique utilizes a spectroscopic or other analytical probe from a number of selections for a broad range of sample systems by employing different types of external perturbations to induce systematic variations in intensities of spectra.Such spectral intensity variations are then converted into2 D spectra by a form of correlation analysis for subsequent interpretation.Many different types of 2D correlation approaches have been proposed.In particular,2D hetero-correlation and multiple perturbation correlation analyses,including orthogonal sample design scheme,are discussed in this review.Additional references to other important developments in the field of 2D correlation spectroscopy,such as projection correlation and codistribution analysis,were also provided.     

Two-dimensional hetero-spectral correlation fluorescence-Raman spectroscopy for a thermotropic liquid-crystalline oligomer

In this paper, 2D fluorescence and 2D hetero-spectral fluorescence-Raman correlation spectroscopies were performed to better understand the dynamic process of liquid crystalline (LC) oligomer, the esterification product of ethyl 4-[4′-oxy-4-biphenyl-carbonyloxy]-4′-biphenylcarboxylate with poly(ethylene oxide)s (PEO) (DP = 12) (designated as 12-4). We found that 2D fluorescence correlation spectroscopy provided much more detailed information on the mechanism of dynamic development of LC oligomer with temperature variation than conventional 1D fluorescence spectroscopy. Furthermore, we investigated the structural change of 12-4 at the molecular level during the phase transitions by using 2D hetero-spectral fluorescence-Raman correlation spectroscopy.     

The roles of carbohydrates, proteins and lipids in the process of aggregation of natural marine organic matter investigated by means of 2D correlation spectroscopy applied to infrared spectra

In this paper the marine organic matter soluble in an alkaline medium called extractable humic substance (EHS), was extracted from three sediment samples of Tyrrhenian Sea and separated by precipitation at pH 2 in the two fractions of fulvic acids (FAs) and humic acids (HAs). FAs were further fractionated in seven sub-samples of different molecular weight (mw) by means of seven different ultrafiltration membranes operating in the range between mw<1 kDa and mw>100 kDa. Then the qualitative composition of each sample of fractionated FAs and HAs was studied by means of one-dimensional Fourier transform infrared spectroscopy in reflectance mode (FTIR-DRIFT) and by two-dimensional (2D) correlation spectroscopy both in wavelength-wavelength (WW) and in sample-sample (SS) mode. The application of 2D correlation WW spectroscopy allows to elucidate the different roles played by carbohydrates and proteins with respect to some lipid compounds such as fatty acids and ester fatty acids during the process of aggregate formations from mw approximately 1 kDa to higher size aggregates. In addition, 2D correlation WW spectroscopy allows to observe some peculiar interactions between carbohydrates and proteins in the formation of EHS aggregates, interactions which vary from a sample to another sample. The results of 2D correlation SS spectroscopy confirm the general evidences obtained by 2D WW spectroscopy and moreover, they also describe the formation of EHS aggregates as a complex process where evolutionary links and connectivity between aggregates of neighbour molecular size ranges are not evident. Two-dimensional correlation spectroscopy applied to FTIR spectroscopy shows to be a powerful tool for the investigation of the mechanisms involved in EHS aggregation because it supports the acquisition of structural information which sometimes can be hardly obtained by one-dimensional FTIR spectroscopy.     

New sesquiterpenes from Euonymus europaeus (Celastraceae)

A new sesquiterpene evoninate alkaloid (1), and two sesquiterpenes (2, 3) with a dihydro-beta-agarofuran skeleton, along with three known sesquiterpenes (4-6), were isolated from the seeds of Euonymus europaeus. Their structures were elucidated by high resolution mass analysis, and one- and two-dimensional (1D and 2D) NMR spectroscopy, including homonuclear and heteronuclear correlation [correlation spectroscopy (COSY), rotating frame Overhauser enhancement spectroscopy (ROESY), heteronuclear single quantum coherence (HSQC), and heteronuclear multiple bond correlation (HMBC)] experiments.     

Advanced solvent signal suppression for the acquisition of 1D and 2D NMR spectra of Scotch Whisky

A simple and robust solvent suppression technique that enables acquisition of high‐quality 1D ¹H nuclear magnetic resonance (NMR) spectra of alcoholic beverages on cryoprobe instruments was developed and applied to acquire NMR spectra of Scotch Whisky. The method uses 3 channels to suppress signals of water and ethanol, including those of ¹³C satellites of ethanol. It is executed in automation allowing high throughput investigations of alcoholic beverages. On the basis of the well‐established 1D nuclear Overhauser spectroscopy (NOESY) solvent suppression technique, this method suppresses the solvent at the beginning of the pulse sequence, producing pure phase signals minimally affected by the relaxation. The developed solvent suppression procedure was integrated into several homocorrelated and heterocorrelated 2D NMR experiments, including 2D correlation spectroscopy (COSY), 2D total correlation spectroscopy (TOCSY), 2D band‐selective TOCSY, 2D J‐resolved spectroscopy, 2D ¹H, ¹³C heteronuclear single‐quantum correlation spectroscopy (HSQC), 2D ¹H, ¹³C HSQC‐TOCSY, and 2D ¹H, ¹³C heteronuclear multiple‐bond correlation spectroscopy (HMBC). A 1D chemical‐shift‐selective TOCSY experiments was also modified. The wealth of information obtained by these experiments will assist in NMR structure elucidation of Scotch Whisky congeners and generally the composition of alcoholic beverages at the molecular level.     

Structure analysis of aromatic medicines containing nitrogen using near-infrared spectroscopy and generalized two-dimensional correlation spectroscopy

Four aromatic medicines (acetaminophen; niacinamide; p-aminophenol; nicotinic acid) containing nitrogen were investigated by FT-NIR (Fourier transform near-infrared) spectroscopy and generalized two-dimensional (2D) correlation spectroscopy. The FT-NIR spectra were measured over a temperature range of 30-130 degrees C. By combining near-infrared spectroscopy, generalized 2D correlation spectroscopy and references, the molecular structures (especially the hydrogen bond related with nitrogen) were analyzed and the NIR band assignments were performed. The results will be helpful to the understanding of aromatic medicines containing nitrogen and the utility of these substances.     

Moving-window two-dimensional correlation infrared spectroscopy study on structural variations of partially hydrolyzed poly(vinyl alcohol)

In the present study, the molecular chain changes and structural transitions of partially hydrolyzed poly(vinyl alcohol) (PVA) having a 12 mol% acetate unit were analyzed by moving-window two-dimensional (MW2D) correlation infrared spectroscopy combined with differential scanning calorimetry and thermogravimetric analysis. The results show the glass-transition temperature (T _g ) of PVA is clearly distinguished by MW2D correlation infrared spectroscopy, and the acetate groups start to be eliminated around the melting temperature, whereas the free water molecules in PVA are eliminated above T _g. The correlation movements of the O–H stretching modes, including the free hydroxyl groups and the hydrogen bonds, are clearly determined using MW2D correlation infrared spectroscopy. The spectral variations in the C=O stretching region caused by the elimination of the acetate unit from polymer chains are also discussed on the basis of the results of the MW2D correlation analysis. Such results cannot be obtained by traditional infrared spectroscopy owing to the complex overlapping peaks.

Adsorption behavior of human serum albumin on ATR crystal studied by in situ ATR/FTIR spectroscopy and two-dimensional correlation analysis

The time-dependent adsorption behavior of human serum albumin (HSA) onto an ATR (ZnSe) crystal was investigated by two-dimensional (2D) correlation analysis and in situ ATR-FTIR spectroscopy following the secondary structural changes in the amide I region. The two major advantages of the generalized 2D correlation spectroscopy were first tested. New extra bands have been resolved by 2D correlation analysis, but they are either artifacts or a result of uncertainty on band position in generalized 2D correlation spectroscopy. The sequence of the intensity variations of the three sub-bands under the amide I band profile deduced from the 'sequential order' rules is contradictory to the experimental observation, which supports our argument on the 'sequential order' rules in generalized 2D correlation spectroscopy (H. Huang, Anal. Chem., 2007, 79, 8281-8292). Subsequent detailed analysis on the in situ ATR-IR spectra shows that the adsorption process of HSA on the ATR (ZnSe) crystal in aqueous solutions can be divided into three stages: no obvious conformational transitions in the first 25 min of adsorption of HSA molecules; large structural rearrangement from α-helix to random coil and short extended chain structures in a fully cooperative way from 25 to 50 min of adsorption; and further slight conformational transformation of short extended chain and turn structures into random coil with no sequential order after 50 min of adsorption.     

Two new pentacyclic triterpenoids from Lantana camara LINN

Two new pentacyclic triterpenoids, namely lantanoic acid (1) and camaranoic acid (2), and six known compounds such as lantic acid, camarinic acid, camangeloyl acid, camarinin, oleanonic acid, and ursonic acid were isolated from the aerial parts of Lantana camara LINN. Structures of the new constituents were elucidated by chemical transformation and spectral studies including 1D ((1)H- and (13)C-NMR) and 2D ((1)H-(1)H correlation spectroscopy (COSY), nuclear Overhauser effect spectroscopy (NOESY), (1)H-(1)H total correlation spectroscopy (TOCSY), J-resolved, (1)H-detected heteronuclear multiple quantum coherence (HMQC), and heteronuclear multiple bond connectivity (HMBC)) NMR spectroscopy.