Sundaresan P Ramnathan, Slavoff Sarah A, Grundel Erich, White Kevin D, Mazzola Eugene, Koblenz Daniel, Rader Jeanne I
Division of Research and Applied Technology, Office of Nutritional Products, Labeling and Dietary Supplements, Food and Drug Administration, 5100 Paint Branch Parkway, College Park, Maryland 20740, USA.
Phytochem Anal. 2006 Jul-Aug;17(4):243-50. doi: 10.1002/pca.912.
Teucrium species, such as germander, are rich in neo-clerodane diterpenoids and have been used in traditional folk medicine for their stimulant, diuretic, antipyretic and antiseptic properties. However, the furano neo-clerodane diterpenoids present in germander have been implicated in the in vivo hepatotoxicity of this botanical. In this study, authenticated germander (Teucrium chamaedrys L. and Teucrium canadense L.) was used as the source material. Methanol extracts of powdered plant mate rial were prepared and analysed by HPLC using Synergi Max-RP columns with monitoring at 220 nm. Limited amounts of teucrin A and other diterpenoid standards were analysed on a Synergi Max-RP column in order to determine their retention times and to generate calibration curves. The same standards were subjected to concurrent mass spectral analysis. Teucrin A and diterpenoids such as dihydroteugin, teuflin, teuflidin and teucvidin were tentatively identified in the plant extracts by HPLC-MS and 1H-NMR experiments. For the isolation of teucrium diterpenoids on a semipreparative scale, a solid-phase extraction method was developed for the first time using styrene divinylbenzene and strata-X sorbents for teucrin A and teuflin, respectively. Semi-preparative HPLC of the methanol extract of the powdered aerial parts of Teucrium plants was carried out on a semipreparative Synergi Max-RP column with photodiode array detection in order to confirm the identities of some diterpenoids by HPLC-MS and NMR.
香科科属植物，如石蚕属植物，富含新克罗烷二萜类化合物，并因其具有兴奋、利尿、退热和防腐特性而被用于传统民间医学。然而，石蚕属植物中存在的呋喃新克罗烷二萜类化合物与该植物的体内肝毒性有关。在本研究中，经鉴定的石蚕属植物（石蚕和加拿大石蚕）被用作原料。制备了粉末状植物材料的甲醇提取物，并使用Synergi Max-RP柱在220 nm波长下进行HPLC分析。为了确定其保留时间并生成校准曲线，在Synergi Max-RP柱上分析了少量的teucrin A和其他二萜类标准品。对相同的标准品进行了同步质谱分析。通过HPLC-MS和1H-NMR实验，在植物提取物中初步鉴定出teucrin A和二萜类化合物，如二氢替鲁因、替弗林、替弗利定和teucvidin。为了在半制备规模上分离香科科二萜类化合物，首次开发了一种固相萃取方法，分别使用苯乙烯二乙烯基苯和strata-X吸附剂分离teucrin A和替弗林。在半制备Synergi Max-RP柱上对香科科植物地上部分粉末的甲醇提取物进行半制备HPLC，并采用光电二极管阵列检测，以便通过HPLC-MS和NMR确认一些二萜类化合物的身份。
