2种颜色拳参饮片HPLC-MS指纹图谱比较研究

Comparative study on HPLC-MS fingerprint of Bistortae Rhizoma prepared slides in 2 different colors

目的:商品拳参饮片有紫红色和棕红色2种颜色,建立拳参饮片HPLC-MS指纹图谱,以了解2种不同颜色的拳参饮片中除绿原酸及没食子酸外,所含其他成分是否异同。方法:采用Inertsil ODS-SP C_(18)色谱柱(4.6 mm×150 mm,5μm),流动相为1%甲酸水溶液(A)^(-1)%甲酸乙腈(B),梯度洗脱,流速0.8 m L·min^(-1),检测波长290 nm,柱温40℃;利用《中药色谱指纹图谱相似度评价系统A版》软件处理分析及多元统计等方法分析,采用高分辨质谱(离子源电离模式:ESI±;加热块温度:200℃;雾化器流量:N2,1.5 L·min^(-1))对部分共有峰进行鉴定。结果:对2种颜色拳参饮片的指纹图谱进行评价,确定了15个共有峰,指认出其中5个峰分别对应为山柰酚、24(E)-亚乙基环木菠萝烷酮-3α-醇、原儿茶酸、绿原酸及没食子酸;比较山柰酚、24(E)-亚乙基环木菠萝烷酮-3α-醇、原儿茶酸、绿原酸4个化学成分的色谱峰面积,紫红色拳参饮片中4个成分色谱峰面积均大于棕红色饮片。结论:本实验建立拳参饮片的HPLC-MS指纹图谱,结果稳定可靠。紫红色与棕红色拳参饮片所含化学成分相似,但主要成分含量存在明显差异。

Objective： To establish HPLC-MS fingerprints of amaranth and brownish red Bistortae Rhizoma prepared slides and to compare their chemical components including chlorogenic acid and gallic acid. Methods： The separation was carried out on a Inertsil ODS-SP C18 （ 4.6 mm × 150 mm, 5 μm ） column with a mobile phase consisting of acetonitrile-water （ containing 1% formic acid ）with gradient elution. The flow rate was 0. 8 mL·min^-1, and the detection wavelength was 290 nm. The column temperature was 40 ℃. The chromatograms were processed by ＂Chinese Traditional Medicine Chromatographic Fingerprint Similarity Evaluation System Edition A＂ and multiple statistical analysis. Part of the common peaks were identified by high resolution mass spectrum （ ionization method： ESI ± ; heat-block temperature： 200 ℃ ; nebulizing gas： N2, 1.5 L· min^-1）. Results： The fingerprints of 2 colors of Bistortae Rhizoma prepared slides were evaluated. 15 common peaks were chosen including kaempferol, protocatechuic acid, 24 （ E ） -ethylidene cycloartane keto-3 α -alcohol, chlorogenic acid and gallic acid. The peak areas of kaempferol, protocatechuic acid, 24 （ E ） -ethylidene cycloartane keto-3 a -alcohol and chlorogenic acid of amaranth slides were bigger than those of brownish red slides. Conclusion： HPLC-MS fingerprint of Bistortae Rhizoma prepared slides was established, and the results were stable. The chemical compositions of the slides in 2 colors were similar, but there were significant differences in major chemical compositions between the amaranth and brown slides.