目的: 建立中药材苣荬菜的高效液相-电喷雾飞行时间质谱(HPLC-IT-TOF/MS)指纹图谱分析方法,为苣荬菜的质量控制、研究开发和应用提供科学依据。方法: 采用Agilent C18色谱柱(250 mm×4.6 mm,5 μm),流动相为0.05%甲酸水溶液(A)-甲醇(B),梯度洗脱,流速为1 mL·min-1,柱温为35 ℃。质谱离子源为ESI源,正离子模式扫描,以氮气为雾化气和干燥气,曲线脱溶剂管及加热模块温度均为200 ℃,检测器电压1.61 kV,扫描范围为m/z 100~1 500。使用“ChemPattern 2020版”软件建立苣荬菜的HPLC-IT-TOF/MS指纹图谱并进行相似度评价,鉴别共有峰,并以市场上常见的易混淆品对所建立方法的有效性进行验证。结果: 建立了苣荬HPLC-IT-TOF/MS指纹图谱,确定了17个共有峰,根据对照品和参考文献指认了5个共有峰。对11批不同来源的样品分别以夹角余弦及相关系数法进行了相似度考察,相似度均大于0.90,易混淆品相似度均小于0.65。结论: 建立了苣荬菜药材HPLC-IT-TOF/MS指纹图谱分析方法,专属性强,可为苣荬菜的真伪鉴别及质量控制研究及其标志物的选择提供参考。
Objective: To establish an HPLC-IT-TOF/MS fingerprint method for the analysis of the whole herbs of Sonchus arvensis to provide scientific basis for the quality control, research and application of S. arvensis. Methods: An Agilent C18 column (250 mm×4.6 mm,5 μm), mobile phase of 0.05% formic acid in water (A)-methanol (B) with gradient elution at a flow rate of 1 mL·min-1 and column temperature of 35 ℃. Mass spectrometry ion source was ESI source, scan in positive ion mode, nitrogen was used as nebulization and drying gas, the temperature of curve desolvation tube and heating module were both 200 ℃, the detector voltage 1.61 kV, scan range was m/z 100~1 500. The HPLC-IT-TOF/MS fingerprint of the whole herbs extract of S. arvensis was established by using “Chempattern 2020” software, the similarity was evaluated, the common peaks were identified, and the effectiveness of the established method was verified by common confusing products in the market. Results: The common mode of HPLC-IT-TOF/MS fingerprint of the whole herbs extract of S. arvensis was established, 17 common peaks were identified, and 5 common peaks were identified according to the reference substance and references. The similarity of 11 batches of samples from different sources was investigated by angle cosine and correlation coefficient method. The similarity was greater than 0.90, and the similarity of easily confused products was less than 0.65. Conclusion: HPLC-IT-TOF/MS fingerprint analysis method of the whole herbs extract of S. arvensis was established, which provided a new method for identification and quality control of the whole herbs extract of S. arvensis, and provided a reference for the selection of quality control markers.
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