川芎中1-(3',4'-二羟基肉桂酰基)环戊烷-2,3-二醇分离鉴定及含量测定

Isolation,Identification and Determination of 1-( 3',4'-dihydroxycinnamoyl)cyclopentane-2,3-diol in Rhizoma Chuanxiong

目的:分离鉴定川芎中指标性成分1-(3',4'-二羟基肉桂酰基)环戊烷-2,3-二醇(DC),并建立其含量测定方法。方法:采用色谱和光谱技术首次从川芎中分离得到DC,采用高效液相色谱法对川芎中DC进行定量分析,Inertsil ODS-3 C18柱(250 mm×4. 6 mm,5μm),流动相:乙腈-0. 05%三氟乙酸水溶液,梯度洗脱,检测波长为325 nm,柱温为30℃。结果:DC的定量测定在0. 023 36～1. 168 0μg(r=1. 000 0)呈良好的线性关系,平均回收率为98. 84%,RSD=1. 45%。结论:该分离方法得到的DC纯度高,可作为含量测定用对照品。建立的定量方法简便、准确、重复性好,可为川芎药材的质量控制提供参考。

Objective： To separate and identify chemical marker 1-（ 3’,4’-dihydroxycinnamoyl） cyclopentane-2,3-diol（ DC） in the rhizomes of Ligusticum chuanxiong and establish an HPLC method for determination the content of DC in Rhizoma Chuanxiong. Methods： DC was separated and identified from Rhizoma Chuanxiong by chromatographic technique and spectroscopic method for the first time. The content of DC was determined by HPLC analysis on an Inertsil ODS-3 C18 column（ 250 mm×4. 6 mm,5 μm） with acetonitrile-0. 05% trifluoroacetic acid aqueous solution as the mobile phase for gradient elution. The detection wavelength was set at 325 nm and the column temperature was 30 ℃. Results： The HPLC method showed good linearity within the range of 0. 023 36-1. 168 0 μg（ r = 1. 000 0） for DC. The average recovery was 98. 84%,and the RSD was 1. 45%. Conclusion： DC obtained by this separation method was with high purity,and it can be adopted as the reference substance. The established quantitative method is simple,accurate and reproducible,and can be used for the quality control of Rhizoma Chuanxiong.