田蓟苷的分离制备与香青兰子药材质量标准研究

Separation and authentication of tilianin and quality standards of semen of Dracocephalum moldavia

该文采用色谱和光谱技术从维药香青兰子中分离并鉴定田蓟苷,经HPLC面积归一法测定其纯度大于98%。采用硅胶SGF254薄层板上,以氯仿-甲醇（5∶1）为展开剂,采用三氯化铝为显色剂,可对香青兰子药材中的活性成分田蓟苷进行定性鉴别。以田蓟苷为指标,采用C18色谱柱（4.6 mm×250 mm,5μm）,以乙腈-0.1%磷酸（25∶75）为流动相,330 nm为检测波长,对香青兰子药材进行定量分析。田蓟苷在0.617 2~123.44 mg·L^-1线性关系良好,标准曲线方程为Y=33.773X-0.824 8（r=1）,平均回收率为101.0%,RSD为3.7%,方法的日内和日间精密度均小于2%。11批香青兰子中的4批正品药材的质量分数在0.016~0.187 mg·g^-1。所建立的定性和定量方法可用于维药香青兰子药材的质量控制。

Tilianin was separated and authenticated from the seeds of Dracocephalum moldavia, a Uygur medicine, by chromato- graphic technique and spectroscopic method. The purity of tilianin is more than 98% determined by HPLC area normalization method. Thin layer chromatography（TLC） method was used to separate tilianin from D. moldavia by mixture of chloroform-methanol（5：1 ） as a developing solvent on high performance silicagel precoated plate （SGF2s4） and using aluminium trichloride as a chromogenic agent for qualitative identification of D. moldavia. To establish a HPLC method for quantitative analysis of D. moldavia, tilianin was used as a quantitative marker and separated on a C18 （4. 6 mm×250 mm, 5 μm） column with acetonitrile-0. 1% formic acid（25： 75） as the mobile phase and detected at 330 nm. The calibration curve of tilianin displayed ideal linearity over the range of 0. 617 2-123.44 μg · mL^-1with a regression equation of Y = 33.773× -0. 824 8 （ r = 1 ）. The average recovery of tilianin was 101.0% with RSD of 3.7%. The RSD values of intra-day and inter-day precision were less than 2%. The content of tilianin in 4 batches of the authenticated semen of D. Moldavia was between 0. 016 and 0. 187 mg · g^-1. The qualitative and quantitative method established is suitable for the quality evaluation and assessment of semen of D. Moldavia.