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目的建立HPLC同时测定钩吻提取物中钩吻素子、钩吻素甲及16-表伏康树卡平碱3种生物碱含量的方法。方法采用YMC C_(18)(250 mm×4.6 mm,5μm)色谱柱,以乙腈和0.025 mol·L~(-1)磷酸二氢钾(磷酸调pH至3.0)水溶液进行梯度洗脱;检测波长为254 nm,柱温30℃进样量10μL,流速1.0 mL·nin~(-1)。结果钩吻素子、钩吻素甲和16-表伏康树卡平碱质量浓度分别在32.2~322、34.4~344、6.2~62μg·m~(-1)内与峰面积呈良好的线性关系,加样回收率分别为98.6%、101.1%、98.3%,RSD分别为1.7%、1.3%、1.1%。结论该方法准确、简便、重现性好,可用于钩吻提取物中钩吻素子、钩吻素甲及16-表伏康树卡平碱的含量测定。
OBJECTIVE To establish a method for the simultaneous determination of three alkaloid contents of crocin, caenorhinol and 16-epi-densaccatine in kou-kou extract by HPLC. Methods A gradient elution was carried out on a YMC C 18 column (250 mm × 4.6 mm, 5 μm) with acetonitrile and 0.025 mol·L -1 potassium dihydrogen phosphate (adjusted to pH 3.0 with phosphoric acid). The detection wavelength Was 254 nm, and the column temperature was 30 ℃. The injection volume was 10 μL and the flow rate was 1.0 mL · nin ~ (-1). Results The mass concentration of hook kinin, pigeon-methyl and 16-epforme karstine in the range of 32.2 ~ 322,34.4 ~ 344,6.2 ~ 62μg · m ~ (-1) showed a good linear relationship with the peak area The recoveries were 98.6%, 101.1% and 98.3%, respectively, with RSDs of 1.7%, 1.3% and 1.1%, respectively. Conclusion The method is accurate, simple and reproducible. It can be used to determine the content of crocin, caenorhinol and 16-epforme of capecitabine in koukou extract.