Determination of Metabolites from Scutellaria baicalensis by GC/MS and 1H NMR

The quality of medicinal herbs and their products is steadily becoming important in tandem with growing interest in complementary alternative medicine for treatment of diseases. Chemical assays with bioactive secondary compounds are usually used for chemical standardization in herbs for quality control purpose. In this study, an analytical platform comprising of a GC-MS technique with an unsupervised multivariate analysis and a complementary one-dimensional ¹H NMR technique was used to obtain the primary metabolite profiling of Scutellaria baicalensis obtained from different medical halls in Singapore. The key primary metabolites such as sucrose, proline, phenylalanine, fructose, and butanedioic acid for the biosynthesis of bioactive secondary metabolites in this medicinal herb were successfully characterized by the combination of the chromatography and spectroscopy techniques. Their results suggested that these compounds could serve as markers for quality control of the herb. The principal component analyses of the GC-MS data reliably discriminated between the various Scutellaria samples indicating that the developed platform was comprehensive and was applicable to assess the quality of other medicinal herbs.     

Phenolic Compounds of Plants of the Scutellaria L. Genus. Distribution, Structure, and Properties

Information on flavones, flavanones, flavanonols, flavonols, chalcones, isoflavones, biflavonoids, lignoflavonoids, and lignane glycosides and stilbenes isolated from plants of the Scutellaria L. genus was systematized and reviewed. A list of 208 phenolic compounds was given according to flavonoid type with an indication of the plant sources, structures, and physicochemical properties and citations of the original articles.     

A Minor New Flavone from Scutellaria baicalensis Georgi

A new flavone,6,2′-dihydroxy-5,7,8,6′-tetramethoxyflavone,was isolated from the roots of Scutellaria baicalensis. Its structure was established on the basis of spectral evidences.     

Purification and preparation of compounds from an extract of Scutellaria barbata D. Don using preparative parallel high performance liquid chromatography

Preparative parallel high performance liquid chromatography combined with solvent partition and other pretreatments were adopted to separate and purify compounds from an extract of Scutellaria barbata D. Don. Mass-triggered fraction collection allowed the rapid and precise isolation of target compounds. Twelve compounds were isolated from the extract of S. barbata D. Don, their purity in area percent was determined by HPLC analysis, and the structures of seven compounds were further identified with HPLC/ESI-MS, (1)H NMR, and( 13)C NMR, among which 4-(3,4-dihydroxy-phenyl)-but-3-en-2-one, acacetin-7-diglucuronide, and luteolin-7-diglucuronide were the first to be identified from this plant. The results demonstrated that multi-channel parallel preparative HPLC/UV/MS is an efficient method for isolation and purification of compounds from natural products.     

Flavonoids of <Emphasis Type="Italic">Scutellaria immaculata</Emphasis> Roots

(±)-5,2′-Dihydroxy-6,7,6′-trimethoxyflavanone, (-)-5,2′-dihydroxy-6,7,8,6′-tetramethoxyflavanone, chrysin, wogonin, apigenin, isoscutellarein, scutellarein, cosmosiin, and the new flavonoid wogonin-7-O-β-D-glucopyranoside, the structure of which was established using chemical transformations and spectral data, were isolated from Scutellaria immaculata roots.__________Translated from Khimiya Prirodnykh Soedinenii, No. 1, pp. 26–28, January–February, 2005.     

黄芩的1H NMR指纹图谱研究

利用PFT-NMR 核磁共振波谱仪测定了黄芩提取物的¹H NMR图谱,对黄芩提取物的¹H NMR指纹图谱进行了解析,并与黄芩苷元、千层纸素A、汉黄芩素和黄芩苷进行了比较,获得了黄芩提取物的特征峰,并利用向量夹角法计算了不同指纹图谱的相似度;结果表明不同黄芩提取物的¹H NMR指纹图谱都显示出黄酮类有效成分特征共振峰,并具有很好的重现性和高度的特征性,可以成为黄芩真伪鉴别的依据;不同黄芩的¹H NMR指纹图谱的相似度计算结果定量地评价了不同指纹图谱的相似性.     

Py-GC/MS分析烟用添加剂黄芩浸膏的热裂解产物

采用在线热裂解气相色谱-质谱法(Py-GC/MS)法研究了黄芩浸膏热裂解行为。在氦气氛围中,将黄芩浸膏分别在300、450、600、750和900℃下进行热裂解,并以GC/MS对其裂解产物进行定性和半定量分析,并用黄芩浸膏进行了卷烟加香试验。结果表明:①黄芩浸膏在这一系列裂解温度下检测到的挥发性热裂解产物分别为12种、19种、40种、55种和46种;②黄芩浸膏低温区(300℃～450℃)裂解后产生大量醛类、酮类、酯类和呋喃类物质,这些物质是构成卷烟香味的重要物质,能改善卷烟吸味、减轻刺激性;③在高温区(750℃～900℃)产生大量的芳香族化合物,如苯、甲苯、乙苯、萘等。该研究为香味物质在卷烟燃烧过程中的挥发性物质提供了例证。     

人工种植黄芩根、茎、叶、花、种子中营养元素的光谱分析

使用火焰原子吸收光谱法对人工种植黄芩的根、茎、叶、花、种子5个部位中的Ca,Cu,Fe,Mn,Zn,K六种矿物元素的含量进行了测定分析。结果表明,黄芩各部位均含有丰富的矿物元素,根中营养元素由高到低的顺序是为Ca>Fe>Cu>Mn>Zn>K,茎中的为Fe>Mn>Zn=Cu>K>Ca,叶中的为Fe>Mn>Zn>Cu>K>Ca,花中的为Ca>Fe>Mn>Zn>Cu>K,种子中的为Ca>Fe>Zn>Mn>Cu>K。研究认为人工种植黄芩茎、叶、花、种子中Fe, Mn, Zn含量皆较高,花和种子中还富含Ca, 根中富含Ca和Fe元素。     

Identifying the chemical markers in raw and wine-processed Scutellaria baicalensis by ultra-performance liquid chromatography/quadrupole time-of-flight mass spectrometry coupled with multiple statistical strategies

Herb processing is a typical pharmaceutical preparation process for traditional Chinese medicine. After processing, its clinical applications and pharmacological effects vary greatly, which is most commonly attributed to the changing chemical properties between raw herb and processed products. In this work, a total of 53 chemical compounds were detected, among which 17 compounds were identified as discriminatory chemicals between raw and wine-processed Scutellaria baicalensis, and 10 components were identified as chemical markers with a cumulative content contribution of 88.75%. In addition, this work revealed that the best wine-processed time was 18 min by investigating the changes of chemical markers in S. baicalensis during processing. This work demonstrated that ultra-performance liquid chromatography/quadrupole time-of-flight mass spectrometry coupled with multiple statistical strategies is an effective approach for screening and identifying discriminatory chemical markers in complex traditional Chinese medicine.     

微波消解-石墨炉原子吸收光谱法测定黄芩中铅

建立了微波消解-石墨炉原子吸收法测定黄芩中铅的方法。在最佳工作条件下,用微波消解处理样品,铅的回收率为97.3%~100.7%,方法的精密度和准确度均能满足检测的要求。