[关键词]
[摘要]
目的 建立蝉蜕Cicadae Periostracum中乙酰多巴胺二聚体A和B的定量分析方法,并用于蝉蜕药材的质量评价。方法 建立HPLC-UV方法,并进行方法学验证,同时对4个基原40批市售药材的2种乙酰多巴胺二聚体进行含量测定,并进行聚类分析。采用优化的Alltima C18(250 mm×4.6 mm,5 μm)色谱柱,乙腈-水流动相,2种成分能与其他色谱峰分开,并达到基线分离,在测定浓度范围内线性关系良好,平均加样回收率在97.53%~102.75%,方法精密度和重复性的RSD均小于5%,样品在24 h内稳定;依据2种乙酰多巴胺二聚体含量进行聚类分析。结果 所建立的分析方法简便,准确度和精密度良好,能作为蝉蜕药材常规定量评价方法;40批蝉蜕药材可聚为3类,但2种乙酰多巴胺二聚体的含量没有基原特征性。黑蚱蝉基原的蝉蜕商品中乙酰多巴胺二聚体的含量差异较大,可能与不同来源的商品污染泥沙的量不同有关。结论 山蝉、华南蚱蝉和蟪蛄基原的蝉蜕含有较高的乙酰多巴胺二聚体,且整体色谱特征与黑蚱蝉基原蝉蜕相似,是蝉蜕药材的潜在资源,严控泥沙应该是保证蝉蜕药材质量稳定一致的主要措施。
[Key word]
[Abstract]
Objective To establish a quantitative method for determining two N-acetyldopamine dimmers (Dimer A and Dimer B) in Cicadae Periostracum (CP), and to quantitatively evaluate the inner quality of CP commercial samples. Methods An HPLC-UV method was developed and validated; The contents of Dimer A and Dimer B in 40 batches of commercial samples derived from four origins were determined and analyzed with hierarchical cluster analysis. Using optional Alltima C18 (250 mm×4.6 mm, 5 μm) column, acetonitrile-water as mobile phase, the two dimers can achieve baseline separation. Good linearity was obtained within the measurement range. The average recoveries were 97.53%-102.75%. And the RSD of precision and repeatability were less than 5% respectively, and the samples were kept stable within 24 h. A total of 40 batches of CP can be divided into three groups with hierarchical cluster analysis. Results The established method is convenient, accurate and precise, and can be used for the inner quality evaluation of CP. The contents of two dimmers were not correlated with the species originated from, and the contents in CP samples derived from Cryptotympana pustulata varied greatly, which maybe owe to the contamination of soil, thus controlling soil residue should be meaningful for the quality consistency of CP. Conclusion The CP samples originated from Auritibicen flammatus, Cryptotympana mandrina and Platypleura kaem pferi also contain higher contents of the two dimmers. Concerning the similar characteristics of the chromatograms with that of Cryptotympana pustulata, the skin of Auritibicen flammatus, Cryptotympana mandrina and Platypleura kaem pferi may be potential resources of CP.
[中图分类号]
R286.2
[基金项目]
国家科技重大专项:中医药优势领域的创新中药关键技术开发研究(2017ZX09301005)