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目的鉴别紫草药材中的萘醌类化合物,建立紫草中3种萘醌类成分的UPLC同时测定方法,比较和分析不同产地紫草中此3种成分的含量,为建立紫草的质量评价方法提供科学依据。方法根据化合物的紫外光谱、液相色谱行为及质谱数据等综合信息鉴别紫草中的萘醌类成分,采用UPLC对紫草中紫草素、乙酰紫草素及β,β′-二甲基丙烯酰紫草素的含量进行测定,流动相为乙腈-0.1%用酸水溶液,检测波长274 nm,流速0.3mL.min-1,柱温35°C。结果对紫草药材中的5种萘醌类成分的化学归属进行了指认,并系统分析了该类成分的质谱裂解规律;测定了紫草药材中的3种紫草萘醌的含量,结果表明,紫草素、乙酰紫草素、β,β′-二甲基丙烯酰紫草素分别在0.98~98,4.40~440,3.07~307.20μg.mL-1范围内线性关系良好(R2=0.9998),平均回收率分别为(n=6)99.84%,102.23%和102.67%。结论紫草中活性成分的识别可以显著增强其质量控制的准确性和专属性,而快速准确的指标成分含量测定方法,也是质量控制的重要检测手段,定性与定量两方面结合,对于紫草药材及其相关产品的质量检测和控制具有重要意义。
OBJECTIVE To identify naphthoquinone compounds in Lithospermum officinale, to establish UPLC simultaneous determination of three naphthoquinones in Lithospermum officinale, to compare and analyze the contents of these three components from Lithospermum officinale in different areas, and to establish the quality evaluation of Lithospermum officinale Methods provide a scientific basis. Methods The naphthoquinone components in Lithospermum alopecuritiforme were identified based on the comprehensive information of UV, LC behavior and MS data of the compounds. UPLC was performed on shikonin, acetyl shikonin and β, β’-dimethyl The content of acryl shikonin was determined. The mobile phase consisted of acetonitrile-0.1% aqueous acid, the detection wavelength was 274 nm, the flow rate was 0.3 mL · min-1 and the column temperature was 35 ° C. Results The chemical assignments of five naphthoquinones in Lithospermum officinale were identified, and the mass spectrometric cleavage rules of these compounds were systematically analyzed. The contents of three kinds of Radix Bupleuri in Rhizoma Compositae were determined. The results showed that , Shikonin, acetylshikonin and β, β’-dimethylacrylshikonin showed good linearity in the range of 0.98 ~ 98,4.40 ~ 440,3.07 ~ 307.20μg.mL-1 respectively (R2 = 0.9998 ), The average recoveries were (n = 6) 99.84%, 102.23% and 102.67%, respectively. Conclusion The identification of the active ingredients in Lithospermum can significantly improve the accuracy and specificity of its quality control, and the rapid and accurate method for determining the content of the index components is also an important means of quality control. Qualitative and quantitative methods are used to identify Lithospermum officinale And related products quality testing and control of great significance.