基于UPLC-Q-TOF-MS/MS技术快速鉴定降香中化学成分

目的:降香为我国传统名贵中药材,然目前市场上降香来源品种复杂,质量差异较大,为进一步明确其药效物质基础,采用超高效液相色谱-串联四极杆飞行时间高分辨率质谱(UPLC-Q-TOF-MS/MS)技术快速分析降香甲醇提取物中的化学成分。方法:采用UPLC RRHD SB-C18色谱柱(3.0 mm×100 mm,1.8μm),以0.1%甲酸水溶液-乙腈为流动相进行梯度洗脱,流速0.3 mL·min^-1,柱温40℃;采用电喷雾离子源,负离子模式采集数据。结果:通过一级精确荷质比和二级碎片信息数据,结合文献资料,质谱裂解规律,Mass bank质谱数据库及对照品的保留时间等,从降香的甲醇提取物中初步鉴定83个化学成分,包括18个黄酮类,31个异黄酮类,10个新黄酮类,9个异黄烷类,7个其他类型黄酮和8个其他类成分。结论:UPLCQ-TOF-MS/MS技术方法可快捷、准确、较全面地鉴定降香甲醇提取物中的化学成分,降香的主要化学成分为异黄酮、黄酮、新黄酮、异黄烷等黄酮类,为降香的药效物质基础研究奠定基础,也为降香药材的质量标准提升提供理论依据和技术支持。

Rapid Identification on Chemical Components in Dalbergiae Odoriferae Lignum by UPLC-Q-TOF-MS/MS

Objective:Dalbergiae Odoriferae Lignum is a rare traditional Chinese medicine material in China.However,there are many varieties of various sources and different qualities in the market at present.In order to further define the pharmacodynamic substance basis,electrospray time-of-flight tandem mass spectrometry(UPLC-Q-TOF-MS/MS)was used to rapidly analyze chemical constituents of methanol extract of Dalbergiae Odoriferae Lignum.Method:Chromatographic separation was performed on an UPLC RRHD SB-C18(3.0 mm×100 mm,1.8μm)for gradient elution,with mixtures of acetonitrile and 0.1%formic acid-water as mobile phases at a flow rate of 0.3 mL·min^-1.The column temperature was maintained at 40℃.The data was collected in a negative ion mode with electro-spray ionization source(ESI).Result:According to molecular ion peaks and MS2 mass spectrometry characteristic fragment ions,Mass Bank databases,as well as the mass spectrometry information of reference substances and relevant literatures,a total of 83 constituents were identified,including 18 flavones,31 isoflavones,10 neoflavonoids,9 isoflavanones,7 other flavonoids and 8 other components.Conclusion:UPLC-Q-TOF-MS/MS can quickly,accurately and comprehensively identify chemical constituents in methanol extract of Dalbergiae Odoriferae Lignum,and isoflavones,flavones,neoflavonoids and isoflavanones are the main chemical constituents,which laid a foundation for the basic research of medicinal substances of Dalbergiae Odoriferae Lignum,and provided theoretical basis and technical support for the improvement of quality standards of Dalbergiae Odoriferae Lignum.