芸香药材中花椒毒素的HPLC测定方法研究

目的:筛选出在芸香中提取花椒毒素的方法,建立HPLC法测定花椒毒素的含量.方法:在避光条件下,利用花椒毒素在二氯甲烷和乙酸溶液中均有较好溶解度,通过二氯甲烷提取,挥干,残渣加5％乙酸溶液溶解,过滤,进样.采用C18色谱柱,流动相为乙腈:0.02 mol·L-1乙酸铵(45:55),流速1.0 mL·min-1,检测波长...

HPLC method for determination of xanthotoxin in Ruta graveolens

Objective:To screen out a method for the extraction of xanthotoxin fromRuta graveolensand to estab-lish an HPLC method for the determination of xanthotoxin content.Methods:In the dark conditions,consideringgood solubility of xanthotoxin in dichloromethane and acetic acid solution,xanthotoxin was extracted by dichlo-romethane and evaporated to dryness.The residue was redissolved with 5%acetic acid solution,filtered and injec-ted to HPLC.The analysis was performed on a C₁₈chromatographic column using a mobile phase of acetonitrile:0.02 mol·L^-1ammonium acetate(45∶55)delivered at a flow rate of 1.0 mL·min^-1.The column temperaturewas 35℃and the detection wavelength was 300 nm.Results:Xanthotoxin showed a good linear relationship in therange of 0.804-80.4μg·mL^-1(r=0.9999),and the average recovery was 96.4%with RSD of 4.0%.The results of 10 batches of samples from different places of production ranged from 0.04%to 0.31%with RSD(n=3)of 0.85%-1.96%.Conclusion:The extraction method of xanthotoxin fromRuta graveolensand HPLC for the de-termination of xanthotoxin have been included in the quality standard(draft)of Ruta graveolens.