Ranieri Tracy L, Ciolino Laura A
Forensic Chemistry Center, US Food and Drug Administration, 6751 Steger Dr., Cincinnati, OH 45231, USA.
Phytochem Anal. 2008 Mar-Apr;19(2):127-35. doi: 10.1002/pca.1025.
Ephedra (ma huang) has been widely used as an herb or herbal extract in both traditional Chinese medicine and Western world dietary supplements. The effects of Ephedra have been attributed to a series of six ephedrine alkaloids including ephedrine and pseudoephedrine. A GC-MS method for the ephedrine alkaloids is described which couples ammoniacal chloroform as the extraction solvent with a two-stage derivatisation scheme. This scheme produces the O-trimethylsilyl, N-trifluoracetyl derivatives (O-TMS, N-TFA) for the primary and secondary amine alkaloids, and the O-TMS derivatives for the tertiary amine alkaloids. Relatively clean extracts are obtained from complex matrices, and the six ephedrine alkaloids are effectively separated and identified. This approach was also evaluated for quantitative analysis, and was shown to provide quantitative results for ephedrine and pseudoephedrine, and good estimates for the four minor alkaloids. Figures of merit are presented for linearity, detection limits, precision and accuracy. We have applied this approach to the rapid screening and profiling of the ephedrine alkaloids in whole Ephedra plants, liquid plant extracts, dried powder plant extracts and a variety of Ephedra-containing dietary supplements.
麻黄（麻黄）在传统中药和西方世界的膳食补充剂中都被广泛用作草药或草药提取物。麻黄的作用归因于一系列六种麻黄碱生物碱，包括麻黄碱和伪麻黄碱。本文描述了一种用于麻黄碱生物碱的气相色谱 - 质谱联用（GC-MS）方法，该方法将氨性氯仿作为萃取溶剂与两步衍生化方案相结合。该方案为伯胺和仲胺生物碱生成O - 三甲基硅烷基、N - 三氟乙酰基衍生物（O - TMS，N - TFA），为叔胺生物碱生成O - TMS衍生物。从复杂基质中获得相对纯净的提取物，六种麻黄碱生物碱得到有效分离和鉴定。该方法还进行了定量分析评估，结果表明其能为麻黄碱和伪麻黄碱提供定量结果，对四种次要生物碱能给出较好的估计值。给出了线性、检测限、精密度和准确度等性能指标。我们已将此方法应用于全麻黄植物、液体植物提取物、干粉植物提取物以及各种含麻黄的膳食补充剂中麻黄碱生物碱的快速筛选和分析。
