毛细管电泳-电致化学发光检测法分离测定中药马尿泡中的托烷类生物碱成分

以铕离子掺杂类普鲁士蓝(Eu-PB)化学修饰铂电极为工作电极,采用毛细管电泳-电致化学发光检测法对4种托烷类生物碱成分（如山莨菪碱、东莨菪碱、阿托品和樟柳碱）进行了分离检测。考察了氧化电位值、运行缓冲液酸度、盐浓度和甲醇含量等实验条件对电泳分离效果及检测灵敏度的影响。在优化的实验条件下,以20 mmol/L的磷酸盐(pH 8.0)-7%(体积分数）甲醇为运行液,各组分在6 min内可达到基线分离,其峰面积的相对标准偏差小于5.0%,迁移时间的相对标准偏差小于1.1% (n=12)。并将该法成功地应用于测定中药马尿泡根茎中的山莨菪碱和东莨菪碱的含量,其含量平均值分别为27.8 g/kg和4.43 g/kg。样品的加标回收率为97.8%～102%。

Determination of tropane alkaloid components in Przewalskia tangutica Maxim. by capillary electrophoresis with electrochemiluminescence detection

Based on an Eu-PB modified platinum electrode as the working electrode, a method for the simultaneous determination of the four tropane alkaloids, anisodamine, scopolamine, atropine and anisodine, by capillary electrophoresis with electrochemiluminescence detection (CE-ECL) has been established. The effects of several factors, such as the detection potential, the acidity and concentration of the running buffer, and the content of the methanol additive were investigated for the improvement of separation ability and detection sensitivity. Under the optimized conditions, these four components could be fully separated from each other in a 20 mmol/L phosphate (pH 8.0) containing 7% (v/v) methanol buffer within 6 min. The relative standard deviations of the peak area and migration time were less than 5.0% and 1.1% (n = 12) respectively for all the four compounds. Thus, the method has been successfully applied to the determination of anisodamine, scopolamine in Przewalskia tangutica Maxim. The average amounts of 27.8 g/kg anisodamine and 4.43 g/kg scopolamine were found in the herbal root-stalk sample. The recoveries of the tropane alkaloids were 97.8% - 102%.