基于准确相对分子质量和多级质谱技术的LC-MS方法鉴定麦冬醇提液中高异黄酮类成分

Identification of homoisoflavonoids in Ophiopogon japonicus alcohol extract by an LC-MS based on precise mass and tandem mass spectrometer

目的建立一种基于准确相对分子质量和多级质谱技术相结合的LC-MS方法,对麦冬醇提液中的高异黄酮类成分进行鉴定。方法色谱分离采用Alltima C18色谱柱(250 mm×4.6 mm,5μm),Alltech保护柱,流动相组成为1 mmol/L乙酸铵水溶液-0.01%乙酸乙腈,梯度洗脱,体积流量为1.0 mL/min,检测波长为298 nm;质谱定性采用飞行时间质谱(TOF/MS)结合离子阱多级质谱(Trap/MSn),负离子模式扫描。结果在麦冬醇提液中,采用TOF/MS筛查出11种成分的分子式,采用Trap/MSn共鉴定出11种成分,并对各峰进行归属。结论两种质谱联用能快速鉴定药材成分,为中药复方复杂体系分析提供了一种有效、可靠的分析模式。

Objective To develop an LC/MS approach based on precise mass and tandem mass spectrometer to identify homoisoflavonoids from Ophiopogon japonicus alcohol extract.Methods Separation was performed on an Alltima C18 reverse-phase column（250 mm × 4.6 mm,5 μm） and an Alltech pre-column.The mobile phase consisted of water containing 1 mmol/L ammonium acetate-acetonitrile containing 0.01% acetic acid was used as gradient elution.The flow rate was 1.0 mL/min.The detection wavelength was 298 nm.A combination of time-of-flight mass spectrometer（TOF/MS） and ion trap tandem mass spectrometer（Trap/MSn） was applied for qualitative analysis under negative ion mode.Results From the alcohol extract of O.japonicus,the molecular formulae of 11 components were screened by TOF/MS and 11 chemical components were identified by Trap/MSn.All of the peaks were attributed.Conclusion This method can be used to identify medicinal ingredients quickly and provide an effective and reliable analytical model,as well as other complex system of traditional Chinese medicine compound.