[关键词]
[摘要]
目的 建立桂枝茯苓胶囊(GFC)中三萜酸类成分UPLC/Q-TOF-MS指纹图谱方法,为评价GFC的质量提供新方法。方法 采用UPLC分离三萜酸类成分,用Q-TOF-MS检测,建立UPLC/Q-TOF-MS指纹图谱。结果 得到灵敏度、选择性和专属性良好的GFC中三萜酸类成分UPLC/Q-TOF-MS指纹图谱,确定了26个共有峰,其中3、5~18、20、23、24共18个峰来自于茯苓,2号峰来自于白芍和牡丹皮,4号峰来自于茯苓、牡丹皮、白芍、桂枝,19号峰来自于牡丹皮、白芍和桂枝,21号峰来自于牡丹皮和白芍,22、25号峰来自于茯苓、牡丹皮、桃仁、白芍、桂枝,26号峰来自于桂枝、白芍、桃仁。10批GFC指纹图谱相似度在0.90以上。UPLC-Q-TOF-MS共鉴定出16个成分,分别为16α-羟基松苓新酸、16α-羟基-栓菌酸、3-酮基-6,16α-二羟基-羊毛甾-7,9(11),24-三烯-21酸、去氢土莫酸、土莫酸、3-酮基-6,16α-二羟基-羊毛甾-8,24-二烯-21酸、依布里酸、猪苓酸C、3-表去氢土莫酸、3-O-乙酰基-16α-羟基松苓新酸、3-表去氢茯苓酸、3-O-乙酰基-16α-羟基-栓菌酸、去氢茯苓酸、茯苓酸、松苓新酸、去氢齿孔酸。结论 该方法准确、快速,具有较好的精密度、重复性和稳定性,适用于GFC的质量控制。
[Key word]
[Abstract]
Objective To construct the fingerprint of the triterpenoic acid in Guizhi Fuling Capsule (GFC) by UPLC/Q-TOF-MS, and give a new method for its quality control. Methods The triterpenoic acid were isolated by UPLC and detected by Q-TOF-MS. The established fingerprint was an atlas of UPLC/Q-TOF-MS. Results The UPLC/Q-TOF-MS fingerprints of triterpenoids in GFC were established, which preserved high precision, selectivity, and specificity. A total of 26 common peaks were selected as the fingerprint peaks of GFC, of which a total of 18 mutual peaks (3, 5—18, 20, 23, and 24) from Poria, peak 2 was from Paeoniae Radix Alba and Moutan Cortex. Peak 4 was from Poria, Moutan Cortex, Paeoniae Radix Alba, and Cinnamomi Ramulus. Peak 19 was from Moutan Cortex, Paeoniae Radix Alba, and Cinnamomi Ramulus, peak 21 was from Moutan Cortex and Paeoniae Radix Alba, peaks 22 and 25 were from Poria, Moutan Cortex, Persicae Semen, Paeoniae Radix Alba, and Cinnamomi Ramulus, peak 26 was from Cinnamomi Ramulus, Paeoniae Radix Alba, and Persicae Semen. The similarity among the 10 batches of GFC was above 0.90. The results of validation met technical requirement of fingerprints. Sixteen chemical components were identified by UPLC-Q-TOF-MS, which were 16α-hydroxydehydrotrametenolic acid, 16α-hydroxychalcic acid, 3-oxo-6,16α-dihydroxy-lanosta-7,9(11),24(31)-trien-21-oic acid, dehydrotumulosic acid, tumulosic acid, 3-oxo-6,16α-dihydroxy-lanosta-8,24-diene-21-oic acid, eburicoic acid, polyporenic acid C, 3-epidehydrotumulosic acid, 3-O-acetyl-16α-hydroxydehydrotrametenolic acid, 3-epidehydropachymic acid, 3-O-acetyl-16α-hydroxyplugymic acid, dehydropachymic acid, pachymic acid, dehydrotrametenolic acid, and dehydroeburicoic acid. Conclusion The method is rapid, accurate, and has desirable precision, reproducibility, and stability, which could be applied to the quality control of GFC.
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[基金项目]
国家"重大新药创制"科技重大专项(2011ZX09101-403)