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目的建立同时测定蝉蜕药材中3种乙酰多巴胺二聚体的含量测定方法,并考察其在药材中的分布。方法利用硅胶柱色谱,开口ODS柱色谱和制备高效液相进行分离纯化,得到3种乙酰多巴胺二聚体,采用超高效液相色谱法(UPLC)对3种乙酰多巴胺二聚体的含量进行测定。结果样品中3种成分的色谱峰能达到基线分离,线性良好。不同部位3种成分的含量差别极大:前螯中3种成分含量最高;腹部含量最低,仅为前螯中含量的1/3;头部和胸部含量相近,约为前螯中含量的1/2。结论所用UPLC法操作简便,结果准确,重现性好,可用于蝉蜕药材中3种乙酰多巴胺二聚体成分的含量测定。鉴于各部分中有效成分的含量差异太大,建议在临床使用过程中,注意药材的完整度,或者取样的均匀度。
Objective To establish a method for the simultaneous determination of three acetyl dopamine dimers in the cicada slough herb and to investigate its distribution in medicinal materials. Methods Three kinds of acetyl dopamine dimers were obtained by silica gel column chromatography, ODS column chromatography and preparative high performance liquid chromatography. The contents of three acetyl dopamine dimers were determined by ultra performance liquid chromatography (UPLC) . Results The chromatographic peaks of the three components in the sample were able to achieve baseline separation with good linearity. The content of the three components in different parts of the extremely different: pre-chelate in the three components highest content; the lowest abdominal content, only pre-chelate content of 1/3; head and chest content similar to pre-chelation content of about 1 /2. Conclusion The UPLC method is simple, accurate and reproducible. It can be used to determine the content of three acetyl dopamine dimers in the cicada sloughs. In view of the significant differences in the content of active ingredients among the various parts, it is advisable to pay attention to the integrity of the medicinal material or the uniformity of sampling during clinical use.