蝉蜕HPLC定量分析方法的建立和质量评价研究  

High performance liquid chromatography method for quantitative evaluation of Cicadae Periostracum

作　　者：曹馨慈 徐金娣[2] 孔铭[2] 周桂荣 何毅 毛茜[2] 李松林[1,2] CAO Xin-ci;XU Jin-di;KONG Ming;ZHOU Gui-rong;HE Yi;MAO Qian;LI Song-lin(Department of Pharmaceutical Analysis,Affiliated Hospital of Integrated Traditional Chinese and Western Medicine,Nanjing University of Chinese Medicine,Nanjing 210028,China;Department of Metabolomics,Jiangsu Province Academy of Traditional Chinese Medicine and Jiangsu Branch of China Academy of Chinese Medical Sciences,Nanjing 210028,China;Skate Key Laboratory of Core Technology in Innovation Chinese Medicine,Tasly Pharmaceutical Group Limited by Share Ltd.,Tianjin 300410,China)

机构地区：[1]南京中医药大学附属中西医结合医院中药质量研究室,江苏南京210028 [2]江苏省中医药研究院中国中医科学院江苏分院中药代谢组研究室,江苏南京210028 [3]天士力医药集团股份有限公司创新中药关键技术国家重点实验室,天津300410

出　　处：《中草药》2020年第7期1909-1913,共5页Chinese Traditional and Herbal Drugs

基　　金：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)。

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,5μm)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。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,5μm)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.

关 键 词：蝉蜕 乙酰多巴胺二聚体A 乙酰多巴胺二聚体B 质量评价 黑蚱蝉 山蝉 华南蚱蝉 蟪蛄 

分 类 号：R286.2[医药卫生—中药学]