目的 建立蟬蛻Cicadae Periostracum中乙酰多巴胺二聚體A和B的定量分析方法，并用于蟬蛻藥材的質(zhì)量評價。方法 建立HPLC-UV方法，并進行方法學(xué)驗證，同時對4個基原40批市售藥材的2種乙酰多巴胺二聚體進行含量測定，并進行聚類分析。采用優(yōu)化的Alltima C₁₈（250 mm×4.6 mm，5 μm）色譜柱，乙腈-水流動相，2種成分能與其他色譜峰分開，并達到基線分離，在測定濃度范圍內(nèi)線性關(guān)系良好，平均加樣回收率在97.53%～102.75%，方法精密度和重復(fù)性的RSD均小于5%，樣品在24 h內(nèi)穩(wěn)定；依據(jù)2種乙酰多巴胺二聚體含量進行聚類分析。結(jié)果 所建立的分析方法簡便，準確度和精密度良好，能作為蟬蛻藥材常規(guī)定量評價方法；40批蟬蛻藥材可聚為3類，但2種乙酰多巴胺二聚體的含量沒有基原特征性。黑蚱蟬基原的蟬蛻商品中乙酰多巴胺二聚體的含量差異較大，可能與不同來源的商品污染泥沙的量不同有關(guān)。結(jié)論 山蟬、華南蚱蟬和蟪蛄基原的蟬蛻含有較高的乙酰多巴胺二聚體，且整體色譜特征與黑蚱蟬基原蟬蛻相似，是蟬蛻藥材的潛在資源，嚴控泥沙應(yīng)該是保證蟬蛻藥材質(zhì)量穩(wěn)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, 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.

R286.2

國家科技重大專項：中醫(yī)藥優(yōu)勢領(lǐng)域的創(chuàng)新中藥關(guān)鍵技術(shù)開發(fā)研究（2017ZX09301005）