摘要
目的建立骨刺胶囊（昆布、骨碎补、白芍、党参等）指纹图谱,并结合质谱信息鉴定特征峰的化学结构信息。方法骨刺胶囊75%甲醇提取液的分析采用Phenomenex Luna C18柱（4.6 mm×250 mm,5μm）;流动相为乙腈-20 mmol/L甲酸铵水溶液体系;体积流量为1.0 m L/min,梯度洗脱;检测波长为254 nm。采用飞行时间质谱（TOFMS）结合离子阱多级质谱（Ion-trap/MSn）,鉴定骨刺胶囊指纹图谱中特征峰的结构,正、负两种离子模式扫描。结果骨刺胶囊HPLC-MS指认21个共有峰,表征昆布、白芍、杜仲、党参、马钱子、鸡血藤、骨碎补、延胡索和桂枝等9味药材的特征成分。以绿原酸为参照物峰,12批样品的相似度在0.821~0.945之间。结论该方法显示,骨刺胶囊主要化学成分相似,质量较稳定。
AIM To establish a fingerprint for analyzing Guci Capsules（ Laminariae thallus eckloniae thallus,Drynariae Rhizoma,Paeoniae Radix alba,Codonopsis Radix,etc.） by HPLC,as well as a combinative LC / MS method for the identification of components in Guci Capsules. METHODS The analysis of 75% methanolic extract of Guci Capsules was carried out on Phenomenex Luna C18column（ 4. 6 mm × 250 mm,5 μm）,with acetonitrile- 20 mmol / L ammonium formate solution as the mobile phase in a gradient elution manner at 1 m L / min for flow rate and 254 nm for detection wavelength. A combination of time-of-flight mass spectrometer（ TOF-MS） and ion trap tandem mass spectrometer（ ion Trap-MSn） was applied for the identification of characteristic peaks under positive and negative ion modes. RESULTS Twenty-one common peaks,representing L. thallus eckloniae thallus,P. Radix alba,E. Cortextheir,C. Radix,S. Semen,S. Caulis,D. Rhizoma,C. Rhizoma and C. Ramulus,were obtained from HPLC chromatograms of Guci Capsules. The similarities of the twelve batches of samples with the referential chlorogenic acid peak ranged from 0. 821 to 0. 945. CONCLUSION This method can show the similar chemical constituents and stable quality of Guci Capsules.
出处
《中成药》
CAS
CSCD
北大核心
2016年第1期98-103,共6页
Chinese Traditional Patent Medicine
基金
国家"重大新药创制"科技重大专项(2014ZX09304307-001-010)
关键词
骨刺胶囊
指纹图谱
高效液相色谱
飞行时间质谱
离子阱多级质谱
Guci Capsules
fingerprint
high performance liquid chromatography（HPLC）
time-of-flight mass spectrometer（TOF-MS）
ion trap tandem mass spectrometer（Ion-trap/MSn）
