大黄炒炭后新生物质的分离鉴定和生成变化规律

目的:分离和鉴定大黄炒炭后新产生的化学成分,并研究其生成变化规律。方法:大黄炭提取液先用大孔树脂富集,用制备色谱分离纯化,通过理化性质及NMR和MS光谱数据确定化合物结构;大黄粉末分别在180,200,220℃烘烤6,8,10,12,14,16,18,20,25,30,35min后,通过HPLC方法测定新生成分的含量。结果:新产生的化学成分为5-羟甲基糠醛,大黄粉末在200℃烘烤炮制12min时,5-羟甲基糠醛含量达到峰值。结论:5-羟甲基糠醛首次从大黄炭中分离得到,可能是大黄炮制的关键指标成分,可以用来控制大黄炭饮片的质量。

Separation and identification of the new chemical constituent from rhubarb charcoal and its formational rule

OBJECTIVE To separate the new chemical constituent from the charcoal of rhubarb after processing and the formational rule of the new compound.METHODS Macroporous resin and preparative chromatography were used to purify and enrich the chemical constituents from the extract of rhubarb charcoal. The structure was determined by NMR and MS spectra. The content of the new compound was determined by HPLC at 180, 200 and 220℃ after the rhubarb powders were roasted for 6, 8, 10, 12, 14, 16, 18, 20, 25, 30 and 35 minutes, respectively.RESULTS The new compound was determined to be 5-hydroxymethylfurfural (5-HMF). The content of 5-HMF reached its peak when the rhubarb powder was roasted for 12 minutes at 200℃.CONCLUSION 5-HMF is separated from rhubarb after processing for the first time. It is a key component of rhubarb processing and can be used to control the quality of rhubarb charcoal.