手性化合物的质谱分析研究

运用不含手性碳的非对称化合物Ｓ－ＢＮＰ酸（Ｓ－ｐｈｏｓｐｈｏｒｓａｅｕｒｅ－（１，１＇－ｂｉｎａｐｈｔｈｙｌ－２，２＇－ｄｉｙｌｅｓｔｅｒ））作反应试剂用快原子轰击反应质谱法（ＦＡＢ－ＲＭＳ）测定手性化合物的绝对构型．发现非对称手性化合物可与不对称手性化合物在质谱中发生立体选择性反应，Ｓ－ＢＮＰ酸可作为一种新的反应试剂来测定手性化合物的绝对构型．     

C_(18)键合相吸附剂富集水中痕量苯并[a]芘

１前言苯并［ａ］芘（ＢａＰ）是多环芳烃（ＰＡＨｓ）类致癌性最强的化合物之一，在饮用水中的含量不得超过０．０１μｇ／Ｌ。用固相萃取（ＳＰＥ）技术富集水样中痕量ＰＡＨｓ的系统研究以前已作过报道［１］，本文选择ＢａＰ为单一目标化合物，重点研究了水样离子强度...     

多胺多羧酸双吡哆醇酯顺磁性金属螯合物及其弛豫性能研究

由二乙三胺五乙酸（ＤＴＰＡ）双酸酐和乙二胺四乙酸（ＥＤＴＡ）双酸酐与维生素Ｂ６族化合物吡哆醇（ＰＮ）或其衍生物合成了一系列新型的多胺多羧酸双吡哆醇酯衍生物及其钆（Ⅲ）、锰（Ⅱ）、铁（Ⅲ）等顺磁性金属螯合物，研究了其中钆（Ⅲ）和锰（Ⅱ）螯合物在体外水溶液中对水质子的纵向弛豫性能（Ｒ１）．结果表明，所有配体和配合物均有很好的水溶性，且对光和空气稳定．螯合物的弛豫率（Ｔ１）可与其母体螯合物相媲美，如钆－二乙三胺五乙酸二吡哆醇酯（ＧｄＤＴＰＡ－ＢＰＮ）和锰－乙二胺四乙酸二吡哆醇酯（ＭｎＥＤＴＡ－ＢＰＮ）的弛豫率Ｒ１分别为５．５和３．１Ｌ·ｍｍｏｌ－１·ｓ－１，与其母体螯合物ＧｄＤＴＰＡ２－和ＭｎＥＤＴＡ２－的Ｒ１值（５．２和２．８Ｌ·ｍｍｏｌ－１·ｓ－１）相当．     

杜衡的化学成分

杜衡（ＡｓａｒｕｆｏｒｂｅｓｉｉＭａｘｉｍ）为马兜铃科（Ａｒｉｓｔｏｌｏｃｈｉａｃｅａ）细辛属植物,又名马辛,为多年生草本植物,产于江苏、安徽、浙江、江西、河南南部、湖北及四）;旧（部［‘］。本品全草入药,具有散风还寒、消痰引水、活血．平喘、定痛等作用Ｉ’１。据报道［’］,其挥发油具有较好的降脂作用,有效成分为一一去枯醇。从杜衡的全草中我们分离鉴定了４个化合物,它们分别为细辛素（１）、卡枯醇（２）、黄樟油素（３）及卜谷奋醇（４）。化合物回白色针晶（石油醚一丙酮）,ｍ．Ｐ．１２１－１２３ｏＣ,Ｃ。…     

化学文摘社和国际科技信息检索网

化学文摘社和国际科技信息检索网张立群（美国化学文摘社，ＣｈｅｍｉｃａｌＡｂｓｔｒａｃｔｓＳｅｒｖｉｃｅ，Ｐ．Ｏ．Ｂｏｘ３０１２．ＣｏｌｕｍｂｕｓＯＨ４３２１０，ＵＳＡ）张曼平（青岛海洋大学化学系，２６６００３）从１９０７年建立以来，化学文摘社（ＣＡＳ...     

乙烯基聚硅氧烷共聚反应竞聚率的测定及其对复合粒子形态的影响

用Ｆｉｍｅｍａｎ－Ｒｏｓｓ法处理数据，测定了乙烯基聚硅氧烷（ＳＶ）与苯乙烯（ＳＴ）、甲基丙烯酸甲酯（ＭＭＡ）和甲基丙烯酸正丁酯（ｎ－ＢＭＡ）的共聚反应的竞聚率，结果为ｒＳＴ＝１．４５和ｒＳＶ＝１．０８，ｒＭＭＡ＝０．７８和ｒＳＶ＝２．０１，ｒｎ－ＢＭＡ＝０．４６和ｒＳＶ＝３．４９．以含ＳＶ的乳液作为种子进行烯类单体的乳液聚合，单体和ＳＶ共聚反应对复合粒子的形态有很大影响。     

拉胀复合物中不同形状包埋体的泊松比的理论分析

１．论文名称　ＰｏｉｓｓｏｎＲａｔｉｏｉｎＣｏｍｐｏｓｉｔｅｓｏｆＡｕｘｅｔｉｃｓ２．发表刊物　Ｐｈｙｓ．Ｒｅｖ．Ｅ，１９９８，５８，６１７３．３．研究者　魏高原（北京大学化学与分子工程学院高分子科学与工程系　北京１００８７１）；ＥｄｗａｒｄｓＳＦ（ＰｏｌｙｍｅｒｓａｎｄＣｏｌｌｏｉｄｓＧｒｏｕｐ，ＣａｖｅｎｄｉｓｈＬａｂｏｒａｔｏｒｙ，ＵｎｉｖｅｒｓｉｔｙｏｆＣａｍｂｒｉｄｇｅ，Ｃａｍｂｒｉｄｇｅ，ＣＢ３０ＨＥ，ＵＫ）４．评介者　童真（华南理工大学材料科学研究所　广州５１０６４１）５．研究工…     

双缓血氨二乙三胺五乙酸酰胺钆,镱螯合物的合成及其弛豫性能

缓血氨（Ｔｒｉｓ，三羟甲基氨基甲烷）修饰多氨多羧酸（二乙三胺五乙酸，ＤＴＰＡ和乙二胺四乙酸，ＥＤＴＡ）得到两种新的双酰胺型氨羧衍生物配体ＤＴＰＡВＴｒｉｓ和ＥＤＴＡＢＴｒｉｓ，并合成了它们的Ｇｄ３＋，Ｙｂ３＋，Ｍｎ２＋，Ｆｅ３＋等顺磁性金属螯合物，研究了Ｇｄ３＋，Ｍｎ２＋和Ｆｅ３＋螯合物作为磁共振成像造影剂的主要性能。结果表明，ＧｄＤＴＰＡＢＴｒｉｓ，ＭｎＥＤＴＡＢＴｒｉｓ和ＦｅＥＤＴＡＢＴｒｉｓ在体外水溶液中对水质子的纵向弛豫率Ｒ１分别为５４，３．１和１．９Ｌ·ｍｍｏｌ－１·ｓ－１，均高于其相应母体螯合物在相同条件下的弛豫率。此外，这些螯合物还具有医用磁共振成像造影剂所要求的高水溶性和化学稳定性。     

化学高考总复习单元练习九 化学实验（B）

化学高考总复习单元练习九化学实验（Ｂ）第Ⅰ卷（选择题，共８４分）一、选择题（每小题３分，每小题只有１个选项符合题意，共１５分）１．在下图装置中，烧瓶是干燥的，烧瓶的位置不得移动，则由Ｂ口进气可收集的气体有（）Ａ．ＮＯＢ．ＳＯ２Ｃ．ＣＨ４Ｄ．ＮＨ３２．...     

聚苯乙炔LB多层膜及其光电导性能的研究

制备了聚苯乙炔（ＰＰＡ）ＬＢ多层膜，将其作为电荷产生层首次应用于机能分离型光电导体领域．从π Ａ曲线发现，ＰＰＡ单分子膜具有表面压力的各向异性和松弛特性．ＴＥＭ照片显示，ＰＰＡ分子链在ＬＢ膜中有序排列．转移比和ＸＰＳ的研究表明，复合膜沉积均匀．与ＰＰＡ涂膜相比，以ＰＰＡ ＬＢ多层膜作为电荷产生层的光电导体表面充电电位Ｖ０＝１３４５Ｖ，光照１ｓ后的光衰百分比ΔＶ１ｓ＝６５０５％，半衰时间ｔ１／２＝０５８ｓ，具有更优异的光电导性能．     

百草元营养包临床应用观察

测定了百草元营养包中含有人体所必需的十四种微量元素和几种宏量元素，从微量元素与保健的角度，观察了百草元营养包补充人体常见缺乏的微量元素和治疗多种常见慢性病的效果，总有效率达89％。     

GC–MS法分析茵陈挥发油成分

采用水蒸气蒸馏法提取茵陈中挥发性成分挥发油,用气相色谱–质谱联用技术(GC–MS)对茵陈挥发油成分进行分析鉴定,并采用峰面积归一化法测定其相对含量。共检出52种挥发性成分,鉴定了其中31种主要挥发性成分,含量较高的组分为石竹素(15.27%)、(–)-斯巴醇(6.64%)、石竹烯(4.89%)等。GC–MS法适用于茵陈挥发性成分的定性分析,具有灵敏度高、分析速度快的特点。     

中医药现代化的支点——分析测试技术与仪器

实现中医药现代化必须采用现代的科学理论和先进的科学技术,方法和手段研究传统中医药。通过分析比较传统中医药和现代医药的研究模式,以及各自的优缺点,提出了中医药现代化的思路和方法,所有这些反映出先进的分析测试技术与大型仪器（HPLC、HPLC－MS、GC、GC－MS、HPCE、IR、UV、NMR、MS和X-ray等)是中医药现代化的有力支点。     

中药药对的化学成分研究——川芎-赤芍挥发油的GC/MS分析

中药药对是复方的最小组成单位,具有中药配伍的基本特点. 药对化学是复方化学的核心内容. 联用色谱和化学计量学方法为中药复杂体系的分离与分辨提供了强有力的工具. 采用GC-MS法分离测定中药药对川芎-赤芍、 单味药川芎和赤芍的挥发油成分,并对其中的重叠色谱峰采用化学计量学解析方法(CRM)进行分辨,得到药对和各单味药的纯色谱曲线和质谱图,药对川芎-赤芍、 单味药川芎和赤芍分别分辨出82,78和57个色谱峰,通过质谱库对分辨的纯组分进行定性,分别得到61,52和33个定性结果,占总含量的90.18%,95.14%和95.82%.     

Utilization of matrix-assisted laser desorption/ionization imaging mass spectrometry to search for cannabis in herb mixtures

Herb mixtures including cannabis among the other herbs have recently appeared. When cannabinoids from herb extracts are detected by chemical examinations such as gas chromatography/mass spectrometry, forensic analysts have to determine whether cannabis is actually in the mixture or the cannabinoids are spiked. Morphological examinations are time-consuming, since it is difficult to find several pieces of cannabis among a large number of herb pieces using a microscope. Here, we propose a procedure for efficiently searching for cannabis in herb mixtures using matrix-assisted laser desorption/ionization imaging mass spectrometry (MALDI/IMS). Pieces of herb mixtures were spread on double-sided adhesive tape attached to a stainless steel plate. The pieces were then covered with a conductive sheet and pressed. After a solution containing a matrix reagent was sprayed, the distribution of cannabinoids in the sample was visualized by MALDI/IMS. Then, just the pieces with cannabinoids could be picked up selectively with tweezers and decolorized. Cystolith hairs and trichomes, which are characteristic of cannabis, were observed in most of these pieces using a biological microscope. This MALDI/IMS procedure enables cannabis to be found in herb mixtures without inefficient random sampling and microscopic morphological examination.     

海南产槟榔、沉香及槟榔-沉香药对中锰的测定与生物利用性

为测定海南产槟榔、沉香及槟榔-沉香(质量比为1∶1)药对中锰的含量与生物利用性,并了解锰的健康效应,采用火焰原子吸收光谱法(FAAS)测定了槟榔、沉香原药及其水煎液中锰的含量,并用体外消化-透析法模拟人体胃肠道消化,研究了锰的生物利用性.结果表明,该法回收率为98.32%～102.40%,RSD为1.24%～1.76%...     

溪黄草微量元素含量及其溶出量分析

用等离子体原子发射光谱法对溪黄草微量元素的含量进行了测定,溪黄草含有１８种元素,其微量元素的水溶出量与溪黄草的提取方法有关。     

Identification of herb Acanthopanax senticosus (Rupr. Et Maxim.) harms by capillary electrophoresis with electrochemical detection.

In this paper, a rapid, high efficient, sensitive and inexpensive approach based on a combination of simple ultrasonic extract and capillary electrophoresis (CE) separation with electrochemical detection (ED), is described to identify herbs by comparing their CE-ED profiles (namely, CE-ED electropherograms). The proposed method takes advantage of ultra-small sample volume, low consumption of organic solvent, simple sample pretreatment and easy cleanup procedure. It was applied to analyze the CE-ED profiles of stems of herb Acanthopanax senticosus (Rupr. Et Maxim.) Harms from different sources and different parts (roots, rhizomes, stems and leaves) of this herb. By comparing peak number, peak height and peak height ratio, we found that the CE-ED profiles showed big differences for the herbs from the different sources and the different parts of this herb. In addition, the distribution of bioactive compounds (isofraxidin, rutin and chlorogenic acid) in the different parts of this herb and their content variations affected by the source were studied with the CE-ED method. Based on their own unique CE-ED profiles, these herbs from the different sources and the different parts of this herb could be easily distinguished. Therefore, the proposed approach could be used as a rapid, high efficient and sensitive method for the identification of herbal medicines.     

Quality assessment of traditional Chinese medicine herb couple by high‐performance liquid chromatography and mass spectrometry combined with chemometrics

This study was designed to develop a simple, specific and reliable method to overall analyze the chemical constituents in clematidis radix et rhizome/notopterygii rhizome et radix herb couple using high‐performance liquid chromatography coupled with tandem mass spectrometry and multiple chemometric analysis. First, the separation and qualitative analysis of herb couple was achieved on an Agilent Zorbax Eclipse Plus C₁₈ column (250 mm × 4.6 mm, 5 μm), and 69 compounds were unambiguously or tentatively identified. Moreover, in quantitative analysis, eight ingredients including six coumarins and two triterpenoid sapogenins were quantified by high‐performance liquid chromatography coupled with tandem mass spectrometry. In terms of good linearity (r² ≥ 0.9995) with a relatively wide concentration range, recovery (85.40–102.50%) and repeatability (0.99–4.45%), the validation results suggested the proposed method was reliable, and successfully used to analyze ten batches of herb couple samples. Then, hierarchical cluster analysis and principal component analysis were used to classify samples and search significant ingredients. The results showed that ten batches of herb couple samples were classified into three groups, and six compounds were found for its better quality control.     

Comparative analysis of main bio‐active components in the herb pair Danshen‐Honghua and its single herbs by ultra‐high performance liquid chromatography coupled to triple quadrupole tandem mass spectrometry

A sensitive, reliable, and powerful ultra‐high performance liquid chromatography coupled to triple quadrupole tandem mass spectrometry method was developed for simultaneous quantification of the 15 main bio‐active components including phenolic acids and flavonoids within 13 min for the first time. The proposed method was first reported and validated by good linearity (r ² > 0.9975), limit of detection (1.12–7.01 ng/mL), limit of quantification (3.73–23.37 ng/mL), intra‐ and inter‐day precisions (RSD ≤ 1.92%, RSD ≤ 2.45%), stability (RSD ≤ 5.63%), repeatability (RSD ≤ 4.34%), recovery (96.84–102.12%), and matrix effects (0.92–1.02). The established analytical methodology was successfully applied to comparative analysis of main bio‐active components in the herb pair Danshen‐Honghua and its single herbs. Compared to the single herb, the content of most flavonoid glycosides was remarkably increased in their herb pair, and main phenolic acids were decreased, conversely. The content changes of the main components in the herb pair supported the synergistic effects on promoting blood circulation and removing blood stasis. The results provide a scientific basis and reference for the quality control of Danshen‐Honghua herb pair and the drug interactions based on variation of bio‐active components in herb pairs.