地黄中环烯醚萜类成分及其氢谱碳谱规律

我们对现有的600多个环烯醚萜类化合物进行比较,认为依据母核的不同,将环烯醚萜类化合物分为5大类便 加合理,地黄中已分得的环烯醚萜类化合物共32个,均属母核为9个碳,且C－10接在C－8上的第Ⅲ类骨架的化合物,本文试图结合已从其它植物中分得的第Ⅲ类骨架的环烯醚萜类化合物的^1H-NMR和^13C-NMR数据,对地黄中所分得的环烯萜类化合物的^1H-NMR和^13C-NMR规律作一总结。     

双黄连口服液的核磁共振氢谱指纹图谱研究

目的:以双黄连口服液为研究对象,建立一种基于核磁共振氢谱(1H-NMR)的指纹识别分析方法。方法:根据口服液样本的特点,以H2O+D2O为溶剂,在25℃下采用预饱和水峰压制脉冲序列noesygppr1d测定20个样本的1H-NMR指纹图谱;对所得图谱的指纹特征进行初步归属,应用主成分分析法对数据进行分析。结果:成功将双黄连口服液20个样本按生产厂家区分开来。结论:1H-NMR指纹识别分析方法可作为中成药指纹图谱研究的辅助方法用于中药质量检测。     

α-(取代苯丙酮酰氨基)-β-取代苯基丙烯酸乙酯化合物的360兆核磁共振氢谱和碳谱

本文由360兆核磁共振仪测定的PMR和CMR谱,结合元素分析、IR及MS等数据,确定了三个未知化学结构的化合物为α-(取代苯丙酮酰氨基)-β-取代苯基丙烯酸乙酯,并归属了全部CMR谱线。由80兆PMR则无法判明。     

茄尼醇的核磁共振谱研究

从烟叶浸膏中提取制备高纯度的茄尼醇，采用gCOSY、gHMQC、gHMBC等技术对茄尼醇的^1H、^13C核磁共振谱信号进行了全归属。     

核磁共振氢谱法(~1H-NMR)测定西他沙星标准物质的含量

目的建立核磁共振氢谱法测定西他沙星标准物质的绝对含量。方法采用Bruker AVANCE-500型和AVANCE-300型仪器,分别以盐酸吉西他滨和齐多夫定为内标,西他沙星中质子信号在δ8.69,δ7.76,δ3.43和δ3.14,盐酸吉西他滨质子信号在δ8.12,δ6.21和δ6.02,齐多夫定中质子信号在δ7.61和δ6.01作为定量峰,0.5 mL DMSO-d6∶氚代盐酸(DCl,44.8mg·L-1)=4∶1为溶剂,测定条件为:探头温度303K,谱宽11.0,中心频率4.9,脉冲序列为zg 30°,延迟时间20s,采样次数32次,窗函数0.3Hz。结果在此条件下,样品与内标盐酸吉西他滨及齐多夫定的定量峰分离良好,进样精密度及重复性较好,线性范围宽,样品与内标盐酸吉西他滨和齐多夫定质量比分别在0.354 9~1.343 9和0.312 4~1.189 2范围内,其线性拟合方程分别为:Y=1.440 9X+0.017 8(r=1.000 0,n=5),Y=1.634 6X+0.008 5(r=0.999 9,n=5)。结果西他沙星的含量分别为99.26%(RSD为0.06%)和99.22%(RSD为0.17%)。结论该方法准确、专属、简便、快速,适用于该药物标准物质的绝对含量测定。     

定量核磁共振氢谱法对徐长卿中丹皮酚含量的快速提取和含量测定（英文）

徐长卿是一种治疗多种疾病的中药材。丹皮酚是徐长卿的主要活性成分,也是质量控制的关键指标物。本文以核磁共振氢谱建立了一种徐长卿中丹皮酚含量的快速、准确、精密的检测方法。结果表明,氘代甲醇作溶剂可以很好的实现核磁共振氢谱中信号的分离,H-6 (δ7.78)可用作定量分析特征信号,均苯三甲酸用作内标。所建立的方法经线性范围、专属性、重复性和稳定性进行了确证。本文首次采用定量核磁共振氢谱检测徐长卿中丹皮酚的含量,线性范围较其他药材中丹皮酚的含量检测更宽。采用单次提取方式对丹皮酚进行提取,方法快速,更利于应用于质量控制中。本文研究表明相对现有基于高效液相色谱检测方法,定量核磁共振氢谱法是一种适合徐长卿质量控制可行的替代方法。     

川芎的氢核磁共振-模式识别法研究

目的 建立鉴别芎真伪的方法.方法 以1HNMR法测定川芎乙醚提取物,将图谱转化为数据矩阵,分别采用PCA、PLS-DA两种模式识别方法分析数据.结果 1HNMR-PCA或1HNMR-PLS-DA两种方法均能有效地区分川芎正品、伪品及次品;后者还能进一步区分川芎与近似品日本川芎.结论 基于全成分的1HNMR-PRA是一种有效的鉴别川芎正品、次品、伪品的新方法,对其他中药药材的鉴别亦具有参考价值.     

定量核磁共振氢谱检测右佐匹克隆片的含量

目的:建立定量核磁共振氢谱(qHNMR)测定右佐匹克隆含量的方法。方法:以1,3,5-三甲氧基苯δ 6.08处质子信号为内标峰,以右佐匹克隆δ 8.54、8.38、8.12、7.78处质子信号为定量峰,以DMSO-d₆为溶剂,在恒温298 K,弛豫延迟时间10 s,扫描次数32次条件下采集氢谱。结果:定量核磁共振氢谱法测定右佐匹克隆片中右佐匹克隆平均含量为2.94%,即平均每片中含右佐匹克隆3.00 mg, RSD为0.15%,与药物说明标示的量基本一致。结论:定量核磁共振氢谱可用于药物中右佐匹克隆含量的测定,并且具有快速、准确以及操作简单等优势。     

氨氯地平和利培酮的1H和13C核磁共振信号归属

目的对氨氯地平和利培酮两种药物分子进行核磁共振研究.方法应用一维和二维核磁共振技术,如gCOSY, gHSQC和gHMBC.结果对两种药物分子核磁共振氢谱和碳谱进行了归属,氟碳间的耦合常数对碳谱的解析提供了有利的证据.结论通过核磁共振化学位移和耦合常数的分析,确证了氨氯地平和利培酮两种药物分子的化学结构.     

Assignments of ^1H and ^13C NMR Signals of Mogroside IVa

Aim To investigate the structure of mogroside IVa isolated from traditional Chinese medicine fructus momordicae [fruits of Siraitia grosvenori (Swingle) C. Jeffery] and summarize the NMR characteristics of the structure. Methods Cormnon extraction, separafion and purification methods were used. Various NMR techniques including ^1H NMR,^13C NMR, DEPT, ^1H-^1H COSY, HSQC, HMBC, NOESY and molecular model simulated by comtmter were used to elucidate the structure. Results ^1H and ^13C NMR signals of mogroside IVa were assigned, and spectroscopic basis was obtained for identification of such type of compounds. Conclusion 1D and 2D NMR techniques including ^1H-^1H COSY, HSQC, HMBC, NOESY spectra are powerful tools for structure analysis. The structure determined by NMR methods is identical with energy minimized conformation simulated by computer.     

罗汉果皂苷Ⅳa碳氢NMR信号的归属

目的　研究传统中药罗汉果的皂苷类化学成分罗汉果皂苷IVa的结构 ,总结其结构的NMR特点。方法　采用常法提取、分离、纯化罗汉果皂苷IVa ,应用NMR方法 ( 1 HNMR、1 3CNMR、DEPT、1 H 1 HCOSY、HSQC、HMBC和NOESY)和计算机分子模拟研究其结构。结果　对罗汉果皂苷IVa的1 H和1 3C信号进行了归属 ,并为该类型化合物的结构确定提供了波谱学依据。结论　包括1 H 1 HCOSY、HSQC、HMBC、NOESY的一维和二维核磁共振波谱技术是对结构进行无创伤性分析的有力工具。NMR方法确定的结构与计算机分子模拟的最优构象一致。     

米菲司酮的^1HNMR及^13CNMR研究

米菲司酮的１ＨＮＭＲ及１３ＣＮＭＲ研究孔漫１）贺文义韩广甸王映红（中国医学科学院中国协和医科大学药物研究所，北京１０００５０）米菲司酮（Ｍｉｆｅｐｒｉｓｔｏｎｅ，ＲＵ４８６）１１β－〔４－（Ｎ，Ｎ－二甲氨基）苯基〕－１７α－（丙炔－１）－Δ４，９－雌...     

Substituted Xanthones as Antimycobacterial Agents,Part 1: Synthesis and Assignment of 1H/13C NMR Chemical Shifts

A series of substituted xanthones was synthesized in order to prove the hypothesis that electron-withdrawing substituents enhance the antimycobacterial activity of these compounds, which is described by means of a QSAR equation with ¹³C NMR chemical shifts as independent parameters. The key step of the synthesis is the formation of substituted 2-phenoxybenzoic acids by Ullmann reaction followed by intramolecular Friedel-Crafts acylation, leading to methyl-, carboxy-, nitro-, cyano-, and aminoxanthones as a test set for QSAR investigations. Spectroscopic data (¹H and ¹³C chemical shifts, IR, UV) of these xanthones are presented and analyzed. Specific shift increments for xanthones depending on the substituent position and on the position of the respective proton/carbon atom as well as additivity rules were developed.     

贝母属植物生物碱的^13C NMR化学位移研究

报道从贝母属植物中分离出的６５个生物碱的＾１３Ｃ ＮＭＲ化学位移数据，并将其进行分类，归纳，指出文献中生物碱的＾１３Ｃ ＮＭＲ化学位移归属存在的错误，阐述生物碱结构不断被修正的必然性，以及用＾１３Ｃ ＮＭＲ谱确定生物碱的结构。     

新药盐酸洛美利嗪的核磁共振谱分析

目的：用核磁共振方法鉴定新药盐酸洛美利嗪的结构。方法：应用HMQC、HMBC等二维核磁共振技术进行测定。结果：对新药盐酸洛美利嗪的^1H-NMR、^13C-NMR谱信号进行了全归属，并测定了其氢氟、碳氟偶合常数。结论：通过二维核磁共振技术确证了新药盐酸洛美利嗪的结构。     

Assignment and conformation of neurotensin in aqueous solution by 1H NMR

A complete assignment of exchangeable and unexchangeable proton resonances of neurotensin 1–13 in aqueous solution has been carried out with the help of its 1–8 and 8–13 fragments. To detect formation of a secondary structure, the effects of peptide fragmentation, temperature decrease, pH changes and addition of denaturing agents on the neurotensin ¹H NMR spectrum were investigated. The small changes observed in all cases support the conclusion that neurotensin exists mainly as a flexible random coiled polypeptidic chain in aqueous solution in agreement with previous CD studies.     

1H and 31P NMR spectroscopy of phosphorylated model peptides

The model peptides glycylglycyltyrosylalanine (Gly-Gly-Tyr-Ala), glycylglycylthreonylalanine (Gly-Gly-Thr-Ala) and glycylglycylserylalanine (Gly-Gly-Ser-Ala) were phosphorylated at the hydroxyl groups of their tyrosyl, threonyl and seryl residues, respectively, and characterized by ³¹P and ¹H NMR spectroscopy. The pK_a-value of the phosphoryl group in the tyrosine-containing peptide determined from the pH dependence of chemical shifts is 5.9, the ³¹P chemical shifts at low pH (4.0) and high pH (8.0) are -3.8 and 0.2 ppm, respectively. Phosphorylation also leads to significant shifts of the ¹H NMR resonances of the tyrosine residue; the amide resonance is shifted -0.02 ppm, the Hα resonance 0.06 ppm, the Hβ resonances 0.10 and -0.04 ppm, the H§ resonances 0.02 ppm and the Hω resonances 0.26 ppm. The pK_a-value of the phosphoryl group in the threonine peptide determined from the pH dependence of chemical shifts is 6.1; the ³¹P chemical shifts at low pH (4.0) and high pH (8.0) are -0.1 and 4.8 ppm, respectively. The corresponding values for the serine peptide are 6.1 (pK_a), 0.6 ppm and 4.9 ppm. Phosphorylation also leads to significant shifts of the ¹H NMR resonances of the threonine and serine residues. In the threonine residue the amide resonance is shifted 0.25 ppm, the Hα-resonance -0.43 ppm, the Hβ-resonance 0.03 ppm and the Hγ-resonance 0.09 ppm. In the serine residue the amide resonance is shifted 0.21 ppm, the Hα-resonance -0.17 ppm, and the Hβ-resonances 0.17 ppm.