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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 C_(18)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 separate and identify the phenolic compounds of Syringa dilatata from the skin of Syringa dilatata, and establish the HPLC method for the determination of syringa glycosides. Methods The compounds were separated and purified by silica gel column chromatography. The structures of the compounds were identified by NMR, MS, UV and IR. The analytical column of Shimpack CLC C_ (18) was used. The mobile phase consisted of methanol-1% acetic acid and eluted with a gradient of 30 ℃. The volume flow rate was 1.0 mL / min and the detection wavelength was 267 nm. Results Two compounds were isolated from the methanol extract of N. crassiphyllum and identified as spectroscopy data for syringin (1) and coniferin (2). The linear range of syringin was 0.2-6.0 mg / mL (r = 0.999 8). The recoveries of syringin were 99.8%, 100.6% and 100.9%, respectively. Quantitative determination of syringin in different parts of the skin showed that the amount in the skin was about 8 times higher than that of the heartwood: and there was no significant difference in the content of syringin in different regions, but in different harvesting periods, the winter systolic was high, Low. Conclusion Two phenylpropanoid phenolic compounds were isolated and identified from North Korea cloves. The established HPLC method has the advantages of fast, simple, high sensitivity, good reproducibility and can be used for the quantitative determination of syringin. For the development and utilization of North Korea clove skin has practical significance.