Smith W M, Clark C C
J Assoc Off Anal Chem. 1976 Jul;59(4):811-6.
Reserpine-rescinnamine group alkaloids are extracted from Rauwolfia serpentina preparations into a dimethylsulfoxide (DMSO)-methanol mixture and diluted with 0.5N H2SO4. The chloroform extract of this solution is passed through a 0.1N NaOH-Celite column and then through a silica gel column. The weakly basic alkaloids trapped on the latter column are eluted with a methanol mixture; a portion of the eluate is treated with nitrous acid and the reserpine-rescinnamine content is determined by measuring the intensity of fluorescence of the oxidation product. The following means and standard deviations (11 collaborators) were obtained for the determination of reserpine-rescinnamine group alkaloids in 4 samples of Rauwolfia serpentina (NF reference powder, 100 mg and 50 mg commercial tablets, and a 45 mg synthetic tablet formulation) : 0.174% +/- 0.0112, 0.131% +/- 0.0047, 0.160% +/- 0.0100, and 0.153% +/- 0.0083, respectively.
利血平-利血胺类生物碱从蛇根木制剂中提取到二甲基亚砜(DMSO)-甲醇混合物中,并用0.5N硫酸稀释。该溶液的氯仿提取物先通过0.1N氢氧化钠-硅藻土柱,然后通过硅胶柱。吸附在后一柱上的弱碱性生物碱用甲醇混合物洗脱;取部分洗脱液用亚硝酸处理,通过测量氧化产物的荧光强度来测定利血平-利血胺的含量。对4种蛇根木样品(美国国家处方集参考粉末、100毫克和50毫克的市售片剂以及45毫克的合成片剂配方)中利血平-利血胺类生物碱的测定得到以下平均值和标准差(11位合作者):分别为0.174%±0.0112、0.131%±0.0047、0.160%±0.0100和0.153%±0.0083。