三七药酒HPLC指纹图谱研究及共有峰LC-MS鉴定

目的：建立三七药酒HPLC指纹图谱，为三七药酒质量评价提供检测方法。方法：采用HPLC方法建立三七药酒的指纹图谱。采用Welch Ultimate XB-C₁₈色谱柱（4.6 mm×250 mm，5-Micron），以乙腈（A）-0.05%乙酸溶液（B）为流动相，梯度洗脱（0~24 min，14% A→20% A；24~40 min，20% A→45% A；40~50 min，45% A→55% A；50~70 min，55% A→65% A；70~75 min，65% A→90% A；75~90 min，90% A），流速1 mL·min^-1，检测波长240 nm，柱温25℃。运用"中药色谱指纹图谱相似度评价系统"对不同季节生产的21个批次的三七药酒进行相似度评价；采用LC-MS对共有峰进行鉴定。结果：建立了三七药酒HPLC指纹图谱，标定了18个共有峰，并结合LC-MS结果，确定了13个峰对应的化合物：原巴西苏木素B、阿魏酸、淫羊藿苷、补骨脂素、异补骨脂素、新补骨脂异黄酮、补骨脂甲素、补骨脂定、藁本内酯、补骨脂乙素、补骨脂二氢黄酮甲醚、补骨脂酚、11-羰基-β-乙酰乳香酸。21批样品相似度在0.994~0.999之间。结论：本文建立的三七药酒指纹图谱对三七药酒质量评价具有指导意义。

Objective: To establish the HPLC fingerprints of Sanqi Yaojiu and to provide a test method for the consistency of the quality.Methods: The fingerprints of Sanqi Yaojiu were established by HPLC.The analysis was performed on a Welch Ultimate XB-C₁₈ column (4.6 mm×250 mm, 5 μm) with gradient elution of acetonitrile (A) -0.05% acetic acid solution (B) (0-24 min, 14%A→20%A;24-40 min, 20%A→45%A;40-50 min, 45%A→55%A;50-70 min, 55%A→65%A;70-75 min, 65%A→90%A;75-90 min, 90%A).The flow rate was 1 mL·min^-1, the detection wavelength was 240 nm and the column temperature was 25℃.Similarities of 21 batches of Sanqi Yaojiu manufactured in different seasons were evaluated by fingerprint system of traditional Chinese medicine and the common peaks were identified by HPLC-DAD-Q-Tof (MS/MS).Results: HPLC fingerprints of Sanqi Yaojiu were established and 13 compounds from 18 common peaks were identified as protosappanin B, ferulic acid, icariin, psoralen, isopsoralen, neobavaisoflavone, bavachin, psoralidin, ligustilide, isobavachalcone, bavachinin A, bakuchiol and 11-keto-beta-boswellic acid, respectively.The similarities of 21 batches of Sanqi Yaojiu were between 0.994-0.999.Conclusion: The fingerprints of Sanqi Yaojiu established in this paper are instructive to the quality evaluation.

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