摘要
目的建立UHPLC/MS^n质谱树技术与Q/TOF联用的方法,对中药复方制剂利舒康胶囊成分进行快速识别和鉴定。方法以含有0.5%乙酸的甲醇-水(3∶1)混合溶液作为提取液制备供试液,采用Thermo Syncronis C_(18)色谱柱(100 mm×2.1 mm,1.7μm)分离,以乙腈-甲醇(1∶1)-0.1%甲酸水溶液为流动相进行梯度洗脱,线性离子阱质谱采用正、负离子同时扫描模式并进行多级质谱碎裂,Q/TOF高分辨质谱分别采用正、负离子扫描模式并进行二级质谱碎裂。结果在线性离子阱正、负离子多级质谱树的验证下,高分辨质谱在中药复方制剂利舒康胶囊中同时确认出生物碱类、黄酮类、三萜类、有机酸类、苯丙素类等各种电离模式下响应的小分子化合物,22个成分经与对照品比对而准确鉴定。结论 UHPLC-Q/TOF高分辨质谱与UHPLC/MS^n质谱树推导技术的联用可以快速鉴定复杂体系中的化学成分,同时也为该复方制剂的质量评价指标选择和药效物质研究奠定了基础。
Objective To develop a method for the rapid identification of the components in Lishukang Capsules with UHPLC/MSn and Q/TOF. Methods The extraction solution was prepared by mixing methanol-water （3 ： 1） and containing 0.5% acetic acid, and the components were separated on a Thermo Syncronis C18 column （100 mm × 2.1 mm, 1.7 μm） with gradient elution using acetonitrile： menthol （1 ： 1, A） and water containing 0.5% acetic acid （B） as mobile phase. Linear ion trap mass spectrometry was performed in the positive and negative ion scan mode simultaneously with acquiring MSn product ion. The Q/TOF high resolution mass spectrometry was performed in the positive and negative ion scan mode respectively and acquiring secondary mass spectrometry fragmentation. Results The constituents were identified by high resolution mass spectrometry combined with the multistage spectral-tree technique. With the standard reference substances, 22 components including alkaloids, flavonoids, triterpenes, organic acids and phenylpropanoids in complex natural products were confirmed. Conclusion The combination of UHPLC-Q/TOF and UHPLC/MSn spectral-tree could rapidly profile the chemical constituents in complex system. This technique also can be used for the quality evaluation and efficacy material research.
出处
《中草药》
CAS
CSCD
北大核心
2017年第10期1944-1956,共13页
Chinese Traditional and Herbal Drugs
