摘要
目的:建立荭草药材中化学成分的超高效液相色谱-电喷雾质谱(UPLC-PDA-ESI/MS)分析方法。方法:采用ACQUITY UPLC系统,BEH C18色谱柱(2.1 mm×100 mm,1.7μm),乙腈-0.1%甲酸水溶液为流动相,流速为0.3 mL.min^-1,梯度洗脱,检测波长190400 nm,柱温45℃。W aters电喷雾三重四级质谱仪,负离子检测模式,ESI喷雾电压3 kV,去溶剂气温度350℃,去溶剂气流量750 L.h^-1(N2),锥孔气流量50 L.h^-1(N2),扫描范围m/z1001 000。结果:荭草中化学成分获得了较好的分离和检测,共鉴定出1个酚酸类成分和11个黄酮类成分。结论:方法灵敏度高、分离度好,适用于荭草药材中化学成分的快速定性鉴定。
Objective: To identify the compounds in herb of Polygonum orientale by ultra-performance liquid chromatography with PDA and electrospray ionization tandem mass spectrometry(UPLC-PDA-ESI/MS).Method: The chromatographic separation was carried out at 45 ℃ on a BEH C18 column(2.1 mm×100 mm,1.7 μm) eluted in the gradient program.The mobile phase consisted of acetonitrile and water containing 0.1% formic acid.The detecion of PDA was set between 190 nm and 400 nm.The mass spectra was obtain by Waters ACQUITYTM triple quadrupole tandem mass spectrometer in negative ion mode with ion spray voltage 3 kV.The temperature of the source and desolvation were set at 120 ℃ and 350 ℃,separately.Nitrogen was used as the desolvation gas(750 L·h-1) and cone gas(50 L·h-1).For collision induced dissociation(CID),argon was used as the collision gas at a flow rate of 0.18 mL·min-1.The mass range recorde,m/z 100-1 000.Result: One phenolic acid,eleven flavonoids were well separated and identified by the method.Conclusion: The method is simple and rapid for the compound identification in the herb of P.orientale.
出处
《中国中药杂志》
CAS
CSCD
北大核心
2011年第1期57-59,共3页
China Journal of Chinese Materia Medica
基金
国家自然科学基金项目(30860366)
国家科技重大专项课题(2008ZX09101-021)
贵州省科技计划重大专项项目(黔科合重大专项字[2007]6010号)