目的 研究铁冬青Ilex rotunda干燥树皮（救必应）的化学成分及其体外抗炎活性。方法 采用硅胶柱色谱、ODS柱色谱、D101大孔吸附树脂柱色谱和半制备高效液相色谱进行分离纯化，并运用HR-ESI-MS、NMR进行化合物结构鉴定。通过测定化合物对脂多糖（lipopolysaccharide，LPS）诱导小鼠RAW264.7巨噬细胞释放炎症介质一氧化氮（NO）的抑制能力，评价化合物的抗炎作用；MTT法测定化合物的细胞毒性。结果 从救必应中分离得到14个化合物，分别鉴定为咖啡酸 [(E)-4-羟基-2-甲基丁-2-烯-1-基] 酯（1）、咖啡酸 [(E)-4-羟基异戊烯基] 酯（2）、咖啡酸(4-羟基异戊烯基)酯 β-D-吡喃葡萄糖苷（3）、rotundarpenoside B（4）、3,5-二咖啡酰基奎宁酸甲酯（5）、3,4-二咖啡酰基奎宁酸甲酯（6）、紫丁香苷（7）、芥子醛葡萄糖苷（8）、di-O-methylcrenatin（9）、咖啡酸（10）、芥子醛（11）、紫丁香醛（12）、原儿茶醛（13）、丁香酸（14）。结论 化合物1和2为2个新的咖啡酸半萜酯，分别命名为咖啡酸半萜酯A和咖啡酸半萜酯B。化合物3的氢谱和碳谱数据为首次报道。化合物1、2和11具有潜在的抗炎活性。

Objective To investigate the chemical constituents from the dried bark of Ilex rotunda (“Jiu Bi Ying” in Chinese) and their anti-inflammatory activities. Methods The compounds of I. rotunda were isolated and purified by silica gel, ODS, D101 macroporous resin column chromatography and semi preparative-HPLC. The structures were elucidated via HR-ESI-MS and NMR spectroscopic data interpretation. The inhibitory rates of the isolated compounds against inflammatory cytokine nitric oxide (NO) production in LPS-stimulated mouse RAW264.7 macrophages were used to evaluate the anti-inflammatory activities. The cell viability was examined by the MTT assay. Results A total of 14 compounds were isolated from the bark of I. rotunda, their structures were elucidated as caffeic acid [(E)-4-hydroxy-2-methylbut-2-en-1-yl]-ester (1), caffeic acid [(E)-4-hydroxyprenyl]-ester (2), caffeic acid [4-hydroxyprenyl]-ester β-D-glucopyranoside (3), rotundarpenoside B (4), methyl 3,5-dicaffeoylquinate (5), methyl 3,4-dicaffeoylquinate (6), syringin (7), sinapaldehyde glucoside (8), di-O-methylcrenatin (9), caffeic acid (10), sinapaldehyde (11), syringaldehyde (12), protocatechuic aldehyde (13), syringic acid (14). Conclusion Compounds 1 and 2 are two new caffeic acid hemiterpenyl esters, named as hemiterpenyl caffeate A and B, respectively. The ¹H and ¹³C NMR spectra of compound 3 are reported for the first time. Compounds 1, 2 and 11 showed potential anti-inflammatory activities.

R284.1

广西中医药大学2020年博士科研启动基金项目（2020BS017）