川西獐牙菜正丁醇提取物的GC-MS成分分析

利用气相色谱-质谱联用技术对川西獐牙菜的正丁醇提取物进行成分分离鉴定,并用峰面积归一法确定各组分的相对含量.实验中从川西獐牙菜正丁醇提取物非沥青质的3种馏分中共分离出122种化学成分,非极性馏分中以烷烃类为主,极性馏分中以饱和脂肪酸类为主.     

野菊花不同提取物的红外光谱分析

利用红外光谱的宏观指纹特性,对野菊花不同溶剂提取物的红外光谱图和二阶导数红外光谱图进行了整体分析。可知,野菊花石油醚提取物主含长链脂肪酸(酯)、不饱和酮以及小分子萜类等低极性化合物,乙酸乙酯提取物主含萜类和黄酮类化合物,无水乙醇提取物主含黄酮及黄酮苷类化合物,95%乙醇提取物主含黄酮苷类化合物,去离子水提取物主含多糖及鞣质类等大极性成分。此外,与野菊花指标成分蒙花苷的红外光谱分析比较,可知野菊花无水乙醇提取物中所含有的黄酮量是最多的。因此,利用红外光谱法对中药提取物直接进行分析,可初步识别其主体成分,为下一步制定药效成分的提取方案和检测方法提供方向性参考。     

傅里叶红外光谱对野生及栽培滇龙胆不同部位的研究

中药及其制剂的应用具有悠久历史,随着研究的深入,市场需求量日益增加,野生资源难以满足市场需求,开展野生和栽培品及化学成分累积动态的研究具有重要意义。为了比较野生和栽培的滇龙胆不同部位(根、茎、叶)化学成分的差异,用傅里叶红外光谱、二阶导数光谱对其进行分析及评价研究。采集60份样品的红外光谱数据,用Nicolet Omnic8.0软件计算各个样品的二阶导数光谱和匹配值。结果显示,野生和栽培滇龙胆根、茎及叶的红外光谱图整体峰形相似,在1 732,1 643,1 613,1 510,1 417,1 366,1 322,1 070cm-1附近主要为酯类、萜类、糖类物质的吸收峰。1 800~600cm-1波段范围内,样品与龙胆苦苷标准品二阶导数光谱的峰位和峰强有差异,具有多个指纹特征峰,分别为1 679,1 613,1 466,1 272,1 204,1 103,1 074,985,935cm-1;野生和栽培样品的根在1 613cm-1(龙胆苦苷中萜类物质C—C吸收峰)附近特征峰明显强于茎和叶,根中龙胆苦苷类成分高于茎及叶;野生样品的茎在1 521,1 462,1 452cm-1附近为木质素类物质的苯环骨架振动峰,并呈现强吸收峰,栽培样品茎呈现中等强峰,茎富含木质素类物质。所有样品红外光谱与野生样品根的平均光谱相似度较大,二阶导数光谱与野生样品根的平均光谱的相关性差异较大,相似度大小分别为:根茎叶。红外光谱法结合二阶导数谱能为同类物种野生和栽培药材不同部位的差异分析和评价提供参考。     

刺五加不同部位的红外光谱分析与鉴定

采用红外光谱三级宏观指纹鉴定的方法对刺五加不同部位根、茎、叶原药材及总苷提取物的红外光谱图进行了整体的分析。原药材谱图显示,根和茎谱图较为相似,主要体现草酸钙和淀粉特征峰,而叶的草酸钙特征峰几乎消失,淀粉特征峰的峰形也变得不明显。总苷提取物的一维谱图显示根、茎、叶在1 602,1 514,1452 cm-1(苯环骨架振动)和1 271 cm-1(CO)附近均有特征吸收,因此,推测三者共有的成分为酚苷类化合物。二阶导数谱图给出叶在1 656 cm-1(黄酮的CO)附近特征峰明显强于根和茎,说明叶中黄酮类成分高于根和茎。二维谱图在1 350～1 700 cm-1波段根和茎均体现苯环骨架振动的5个自动峰1 636, 1 600,1 521,1 462,1 453 cm-1,叶除了苯环骨架振动峰外还出现1 656 cm-1黄酮类成分的CO振动,进一步证实叶中黄酮类成分高于根和茎。     

金银花不同提取物的红外光谱

利用红外光谱的宏观指纹特性,对金银花中不同溶剂提取物的红外光谱图和二阶导数红外光谱图进行了整体分析.初步推测,金银花石油醚提取物中主含长链脂肪酸(酯)、小分子萜类等低极性化合物,乙酸乙酯提取物主含环烯醚萜及其苷类化合物,无水乙醇和95％乙醇提取物中主含咖啡酸类衍生物和黄酮(苷)类化合物,去离子水提取物中主含鞣质及多糖类成分.综合比较亦可知,金银花醇提取物中的主成分是以绿原酸为代表的咖啡酸类衍生物.可见,利用红外光谱法对中药提取物直接进行分析,可对其主体成分进行初步的识别,为制定下一步的提取方案和检测方法提供了方向性参考.     

黄芩及其提取物红外光谱与二维相关光谱的鉴别

采用二维红外相关技术,对黄芩原药材、饮片及其提取物进行分析研究。在一维红外光谱中,各样本间的谱图十分相似,导数光谱分析发现,经过炮制之后在1 745和1 411 cm-1处吸收峰向高波数位移,1 357 cm-1处吸收峰向低波数位移。二维红外谱图显示的药效组分特征差异明显,生黄芩在1 300～1 800 cm-1波数范围内有4个特征峰,以1 575 cm-1最强;黄芩片的自动峰有3个区域;酒黄芩的自动峰有2个区域。各区域内自动峰均为正相关。不同样品总苷提取物的一维谱图显示, 在1 615, 1 585, 1 450 cm-1(苯环骨架振动)和1 658 cm-1(CO)附近均有特征吸收,二阶导数谱图给出在1 656 cm-1(黄酮的CO)附近有特征峰,推测共有的成分为酚苷类化合物。二维谱图在800～1 800 cm-1波段均体现苯环骨架振动的5个自动峰1 366,1 420,1 508,1 585,1 669 cm-1。可见红外光谱宏观指纹技术可提供大量整体信息,能够较准地把握黄芩的整体质量。可用于研究黄芩药材及饮片特征的相关性。     

三种石斛及其提取物的红外光谱法整体结构解析与鉴定

运用红外光谱法对铁皮石斛、金钗石斛、鼓槌石斛及其两种提取物所含化学成分的红外谱图整体变化规律进行解析和鉴定。采用傅里叶变换红外光谱对三种石斛及其提取物进行结构分析及鉴别。原药材粉末一维红外光谱图反映出铁皮石斛、金钗石斛和鼓槌石斛均含有2 920,2 852,1 737和1 509 cm-1附近的特征峰;1 000~1 200 cm-1波段内的特征峰,推测三种石斛均含有脂类、芳香类和淀粉类成分。二阶导数谱进一步佐证了以上结果。根据峰强来判断三种石斛所含化合物含量的差别,得出铁皮石斛和金钗石斛中的脂类和淀粉类成分含量较鼓槌石斛高,三者中以金钗石斛的脂类成分、铁皮石斛的多糖成分含量较高。三种石斛原药材粉末二阶导数光谱中观察到1 318和782 cm-1处草酸钙的吸收峰。三种石斛的两种提取物中的成分种类和含量与其原药材均有所不同,且不同种石斛之间也存在峰形、峰位、峰强的差别。在水提醇沉提取物、无水乙醇提取物中均发现油脂类、芳香类和多糖类成分的特征吸收峰。与标准品比对分析发现,金钗石斛和鼓槌石斛的多糖成分以淀粉为主,而铁皮石斛则以黏多糖为主;三种石斛无水乙醇提取物的红外光谱分析更清楚地发现脂类成分和芳香类成分的存在,且脂类成分以金钗石斛提取物的含量相对较高。芳香类成分以鼓槌石斛提取物的含量相对较高,红外光谱整体结构解析与鉴定方法能够递进式地验证铁皮石斛、金钗石斛和鼓槌石斛所含物质结构和量的差异,适合于不同种石斛的快速鉴别及质量评价与控制。     

七种不同产地仙鹤草原药材及提取物的红外光谱与二维相关红外光谱的分析与鉴定

采用红外光谱、二阶导数红外光谱以及二维相关红外光谱,对七种不同产地的仙鹤草原药材及其总鞣酸提取物进行了鉴别分析。仙鹤草原药材的红外光谱中出现了1 151,1 101,1 032 cm-1的淀粉特征峰,同时还出现了1 618,1 318,780 cm-1的草酸钙特征峰,说明在原药材粉末中同时有淀粉和草酸钙存在。原药材丙酮提取物中所含淀粉等基本成分大为减少,而总鞣酸等有效成分的相对含量增加,因此不同产地仙鹤草丙酮提取物的红外光谱中均出现1 711与1 447 cm-1的鞣酸特征峰。应用红外光谱、二阶导数红外光谱以及二维相关红外光谱技术,不仅可以提供仙鹤草主要化学成分的相关信息,还可以对不同产地的仙鹤草药材进行很好的区分。因此红外光谱法是考察中药资源的一种快速、准确、有效的方法。     

大血藤药材及不同提取物FTIR的比对分析

采用红外光谱法(FTIR)、二阶导数红外光谱法和二维相关光谱分析技术(Two-Dimensional Correlation Spectroscopy) 对江西和安徽大血藤药材、水提物、蒽醌类提取物和残渣进行了快速无损比对分析研究,从中发现两产地大血藤药材的谱图中均出现1 400～1 620 cm-1和1 000～1 200 cm-1两个强峰带,说明药材含有大量的药效成分蒽醌类和糖类物质;蒽醌提取物的谱图中也有上述2个谱带,但1 400～1 620 cm-1谱带明显强于1 000～1 200 cm-1谱峰,说明该提取工艺适宜提取蒽醌类物质;而水提物中2个谱峰带则是后者明显强于前者,证实该提取工艺适宜提取糖类物质;另外通过红外谱图和二阶导数红外谱图的对比发现在药材残渣中含有大量的草酸钙晶体。证明红外光谱技术不仅能对原药材及提取物的药效基团进行分析和指认,还能区分不同产地药材的提取物含量的高低,成功地建立了大血藤及其不同提取物药效成分比对分析的新方法。     

短瓣金莲花不同提取部位的红外光谱分析

利用红外光谱的宏观指纹特性,对短瓣金莲花不同溶剂提取部位的红外光谱图和二阶导数红外光谱图进行了整体分析.综合分析可知,短瓣金莲花石油醚提取部位主含长链烷烃、脂肪酸或酯类成分,乙酸乙酯提取部位主含长链脂肪酸（酯）及黄酮类化合物,95％乙醇提取部位主含黄酮及黄酮苷类化合物,60％乙醇提取部位主含黄酮苷及多糖类成分,30％乙醇和去离子水提取部位主含多糖类成分.因此,利用红外光谱法可从整体上对中药不同提取部位的主体成分进行直接、快速的分析,为中药提取物的工艺优化及其分析研究提供有价值的参考和方向性指导.     

The Fundamental Bands in the Infrared Spectrum of Stibine (SbH3)

The infrared spectrum of stibine, SbH₃, has been recorded in the regions between 720 and 1000 cm^-1 and between 1750 and 2020 cm^-1 at a resolution of about 0.004 cm_-1. Rovibrational transitions belonging to the ν₂, ν₄ bending and ν₁, ν₃ stretching fundamental bands have been measured and assigned for both ¹²¹Sb and ¹²³Sb isotopomers. Strong perturbations due to rovibrational interactions have been observed both in the bending and in the stretching bands. Splittings of the K″=3, 6, and 9 lines have been observed and perturbation-allowed transitions with selection rules Δ (k−?)=±3, ± ±6, and ±9 have been also identified. Simultaneous analyses of transitions belonging to the ν₂/ν₄ or ν₁/ν₃ dyads have been performed. The central frequencies of the hyperfine structures of the rotational transitions in the v₂=1 and v₄=1 states, recorded in the microwave region by Fourier transform spectroscopy [H. Harder, C. Gerke, and L. Fusina, J. Chem. Phys.114, 3508-3523 (2001)], have been included in the data set. The theoretical model adopted explicitly takes into account the Coriolis interactions between the v₁=1 (A₁) and v₃=1 (E) and between the v₂=1 (A₁) and v₄=1 (E) states, including also several essential resonances within them.     

The ν1, ν2, and ν3 Band Systems of 3-Isocyano-2-propynenitrile (NCCCNC): Comparison with the ν4 System of Dicyanoacetylene

The hot bands in the ν₁, ν₂, and ν₃ band systems of NC-CC-NC (3-isocyano-2-propynenitrile) have been investigated and transitions from nv₉-levels with n up to 4 have been identified. Two weak bands have also been observed in the gas phase infrared spectrum at 2157 and 2410 cm⁻¹, of which the latter is probably 2v₄. A preliminary investigation of some analogous hot bands in the v₄ band system of the related molecule NC-CC-CN (dicyanoacetylene) is also reported.     

硬脂酸亚甲基面内摇摆振动二维红外光谱研究

在293~393K温度范围内,分别采用一维红外光谱、二阶导数红外光谱和二维红外光谱测定硬脂酸亚甲基面内摇摆振动(ρCH2)。实验发现:在700~750cm-1范围内,硬脂酸ρCHα存在"第一特征谱带"和未见文献报道的"第二特征谱带"。并进一步研究了温度对于硬脂酸ρCH2红外吸收强度及变化顺序的影响。     

Synthesis,Structural and Optical Studies of Barium Strontium Titanate Borosilicate Glasses Doped with Ferric Oxide

Various barium strontium titanate borosilicate glasses were prepared by a rapid melt-quench technique. Spectroscopic studies have been carried out on investigated glasses for their structural information. Infrared and Raman spectroscopic studies showed that these glasses are formed by glass-forming network of borate and silicate as well as network modifiers in the form of cations of alkaline earth atoms. The borate and silicate networks are modified by barium, strontium, titanium, and iron cations in glass matrix. The network of triborate unit is modified in tetraborate unit by adding ferric oxide in a glassy matrix. The optical studies are performed by ultraviolet-visible spectroscopy and it confirms that the band gap decreases with increase in the concentration of ferric oxide.     

自然老化谷类种子的二维红外光谱研究

种粮老化影响种子活力及粮食品质。利用傅里叶变换红外光谱(FT-IR),二阶导数红外光谱(SD-IR)和二维相关红外光谱(2D-IR)方法对不同储藏年份的大麦,小麦,稻谷,玉米和高粱种子进行区分研究。结果显示,原始光谱中几个峰强比有差异;在二阶导数红外光谱中,不同储藏年份种子在1 800～800 cm-1范围内的吸收峰强度和形状显示出差异。二维相关红外光谱结果显示：大麦在1 350～1 800 cm-1,小麦,稻谷,玉米和高粱在860～1 690 cm-1范围内有明显差异,随储藏年份增加,自动峰和交叉峰的数目减少,强度减弱。结果表明,应用傅里叶变换红外光谱结合二维相关红外光谱能有效快速地区分不同储藏年份的谷类种子。     

Study of the Fundamental Bands of GeD4 by High-Resolution Raman and Infrared Spectroscopy: First Experimental Determination of the Equilibrium Bond Length of Germane

The four fundamental bands of ⁷⁰GeD₄ have been analyzed using the STDS software developed in Dijon (http://www.u-bourgogne.fr/LPUB/sTDS.html). Both infrared and Raman spectra were used to observe all fundamental bands. Infrared spectra of monoisotopic ⁷⁰GeD₄ were recorded in the regions 600 and 1500 cm⁻¹ using the Bruker 120HR interferometer at Wuppertal. The resolution (1/maximum optical path difference) was between 2.3 and 3.3×10⁻³ cm⁻¹ for the ν₃ and ν₄ infrared-active fundamental bands as well as for the interacting ν₂ band. A high-resolution stimulated Raman spectrum of the ν₁ band has been recorded in Madrid. The instrumental resolution of the Raman spectrum was 3.3×10⁻³ cm⁻¹. We have performed a global fit of the ground state, ν₂/ν₄ bending dyad, and ν₁/ν₃ stretching dyad. We have used 1146, 139, and 676 assigned lines for ν₂/ν₄, ν₁, and ν₃, respectively. The standard deviation is 2.2×10⁻³ cm⁻¹ for the bending dyad, 1.6×10⁻³ cm⁻¹ for the ν₃ infrared lines, and 1.7×10⁻³ cm⁻¹ for the ν₁ Raman lines. These results enabled us to perform the first experimental determination of the equilibrium bond length of germane as r_e=1.5173(1) Å.     

泡沫红外消光影响因素的实验研究

通过红外光谱实验和红外热成像实验,研究了影响泡沫红外消光的因素,结果表明:泡沫溶液的红外光谱特征决定红外光谱吸收峰位,且溶质浓度越高,吸收越强;泡沫结构是造成光线强烈衰减的重要原因,透射光强随光线穿过泡沫液膜界面的次数成指数衰减,泡沫直径越小,达到相同遮蔽效果的泡沫溶液的用量就越少;当泡沫直径远大于入射光线波长时,透射比随光束大小变化不大;泡沫溶液升温可在一定程度上增强泡沫的红外吸收强度.各因素影响程度从大到小的次序为:泡沫结构,红外光谱特征,内充气体折射率,泡沫直径,温度.     

Polymorphism incidence in commercial tablets of mebendazole: a vibrational spectroscopy investigation

Mebendazole is a broad spectrum anthelminthic drug, which is widely used in large scale deworming programmes. This active pharmaceutical ingredient exhibits three crystal forms, namely, polymorphs A, B, and C. Therapeutic trials suggested that the most stable form, polymorph A, is inactive. However, the dissolution test normally used as a quality control tool is not able to discriminate among the polymorphs of mebendazole. In this work, the ability of the vibrational spectroscopic techniques (mid and nearinfrared absorption and Raman scattering) for the identification of the crystal form of this compound is evaluated. On the basis of these observations, this methodology is applied to determine the polymorphs of MBZ used in the formulation of the commercial tablets available in the Brazilian and German markets. Copyright © 2008 John Wiley & Sons, Ltd.