目的 从朝鲜丁香Syringa dilatata皮中分离出苯丙素酚类成分并进行结构鉴定, 建立测定紫丁香苷的HPLC分析方法。方法 采用硅胶柱色谱法进行分离纯化, 通过NMR、MS、UV和IR等方法鉴定化合物的结构。使用Shimpack CLC C₁₈分析柱, 流动相为甲醇-1%醋酸, 梯度洗脱, 柱温为30 ℃, 体积流量为1.0 mL/min, 检测波长为267 nm。结果 从朝鲜丁香皮甲醇提取物中分离得到2个化合物, 经波谱数据鉴定为紫丁香苷(1)和松柏苷(2)。测得紫丁香苷的线性范围为0.2～6.0 mg/mL(r=0.999 8), 加样回收率为99.8%、100.6%、100.9%。不同部位中紫丁香苷定量测定结果表明, 皮中的量均高于心材约8倍;而且不同的地区紫丁香苷的量没有明显差异, 但在不同采收期表现为冬季偏高, 暑季偏低。结论 从朝鲜丁香中分离鉴定了2个苯丙素酚类化合物。建立的HPLC法操作快速、简便、灵敏度高、重现性好, 可使用于紫丁香苷的定量测定。对于开发利用朝鲜丁香皮具有现实意义。

Objective To isolate phenyl propanoides from the barks of Syringa dilate, identify their structures, and determine the contents by reliable HPLC. Methods Phenyl propanoides were extracted with methanol, and isolated by silica gel chromatography. The structures were elucidated by spectroscopic analysis including NMR, MS, UV, and IR. Shimpack CLC C₁₈ (150 mm × 6 mm, 5 μm) column chromatography was employed with gradient elute of 1% acetic acid and methanol, and the column temperature was set at 30 ℃. The flow rate was 1.0 mL/min and the detection wavelength was set at 267 nm. Results Two phenyl propanoides were isolated from the barks of S. dilata grown in DPR of Korea and identified as syringin (1) and coniferin (2). The linear range of syringin was 0.2—6.0 mg/mL, the correlation co-efficient was 0.999 8, and the average recoveries were 99.8%, 100.6%, and 100.9%. The results showed that the content in the barks was 8 folds of inner parts. There was no difference in locations and the content of syringin increased in winter, while decreased in summer. Conclusion The elucidation of phenyl propanoides existence in S. dilata could be a fundamental for the search of new herbal materials. The method is simple, rapid, and reliable. It can be used to determine the content of syringin in herbal medicines.