Carlson M, Thompson R D
U.S. Food and Drug Administration, Minneapolis, MN 55401, USA.
J AOAC Int. 1997 Sep-Oct;80(5):1023-8.
A liquid chromatographic (LC) method was developed for determining safrole in herbal products derived from sassafras (Sassafras albidum), as well as related compounds such as isosafrole and dihydrosafrole. The procedure involves solvent extraction and isolation of analyte by reversed-phase LC with UV detection at 235 nm. Safrole is resolved from related compounds and other sample constituents including thymol, a component of thyme. A linear concentration range of 0.003-0.200 mg/mL was obtained for safrole, isosafrole, and dihydrosafrole. Limits of detection (LOD) and quantitation (LOQ) were e0.0015 and 0.0051 micrograms/mL for safrole, 0.0018 and 0.0061 micrograms/mL for isosafrole, and 0.0038 and 0.0125 micrograms/mL for dihydrosafrole, respectively. Intraday relative standard deviations (RSDs) for safrole (n = 5) from various samples ranged from 1.30 to 5.39% at analyte levels of 0.01-1.5%. Safrole contents of 26 samples including root bark powder, leaves, oils, tea concentrate, herbal extract tinctures, and herbal powder capsules ranged from < LOD for most leaf samples to 92.4% for an oil. Recoveries of safrole from fortified samples ranged from 83.6% for an oil to 117.2% for a tincture preparation. Safrole contents of 0.09-4.66 mg/cup were found for brewed teas prepared from sassafras root bark powders and tinctures.
开发了一种液相色谱（LC）方法，用于测定源自美洲檫木（Sassafras albidum）的草药产品中的黄樟素，以及异黄樟素和二氢黄樟素等相关化合物。该程序包括溶剂萃取，并通过反相LC在235 nm处进行紫外检测来分离分析物。黄樟素与相关化合物以及其他样品成分（包括百里酚，百里香的一种成分）得以分离。黄樟素、异黄樟素和二氢黄樟素的线性浓度范围为0.003 - 0.200 mg/mL。黄樟素的检测限（LOD）和定量限（LOQ）分别为0.0015和0.0051微克/毫升，异黄樟素为0.0018和0.0061微克/毫升，二氢黄樟素为0.0038和0.0125微克/毫升。在0.01 - 1.5%的分析物水平下，来自各种样品的黄樟素日内相对标准偏差（RSD）（n = 5）范围为1.30%至5.39%。26个样品（包括根皮粉、叶子、油、茶浓缩液、草药提取物酊剂和草药粉胶囊）中的黄樟素含量，大多数叶子样品低于检测限，一种油中的含量为92.4%。加标样品中黄樟素的回收率范围为，油为83.6%，酊剂制剂为117.2%。用美洲檫木根皮粉和酊剂制备的冲泡茶中，黄樟素含量为0.09 - 4.66 mg/杯。
