芸香药材中花椒毒素的HPLC测定方法研究  

HPLC method for the determination of xanthotoxin in Ruta graveolens

作　　者：周钢 马方圆 单莲莲 蔡阳 柴冰阳 沙拉麦提·艾力 张军[3] ZHOU Gang;MA Fangyuan;SHAN Lianlian;CAI Yang;CHAI Bingyang;SALAMET Aili;ZHANG Jun(Xinjiang Uygur Autonomous Region Drug Inspection and Research Institute;NMPA Key Laboratory for Quality Control of Traditional Chinese Medicine(Uyghur)Medicine,Urumqi 830054,China;Chinese Pharmacopoeia Commssion,Beijing 100061,China)

机构地区：[1]新疆维吾尔自治区药品检验研究院 [2]国家药品监督管理局中药(维药)质量控制重点实验室,乌鲁木齐830054 [3]国家药典委员会,北京100061

出　　处：《中国药品标准》2022年第1期55-58,共4页Drug Standards of China

基　　金：国家食药监督总局药化注册司专项子项目“特色民族药材检验方法的示范性研究”(第2期)。

摘　　要：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C_(18)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300 nm,柱温35℃。结果:花椒毒素在0.804~80.4μg·mL^(-1)范围内线性关系良好(r=0.9999);平均加样回收率为96.4%,RSD=4.0%。不同产地的10批样品测定结果为:0.04%~0.31%,RSD(n=3)为0.85%~1.96%。结论:本实验建立的芸香中提取花椒毒素的方法及HPLC法能有效地测定芸香中花椒毒素的含量,本法已列入芸香药材质量标准(草案)。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 C_(18)chromatographic column using a mobile phase of acetonitrile:0.02 mol·L^(-1)ammonium 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.

关 键 词：芸香 花椒毒素 提取方法 HPLC 含量测定 

分 类 号：R921.2[医药卫生—药学]