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目的建立桂枝茯苓胶囊(GFC)三萜类成分UPLC指纹图谱方法,为评价GFC的质量提供新方法。方法采用Agilent Zorbox Eclipse Plus HD C18(100 mm×2.1 mm,1.8μm)色谱柱,以乙腈-0.1%磷酸水溶液为流动相,梯度洗脱,体积流量0.2 m L/min,柱温30℃,检测波长为210 nm。采用Q-TOF/MS对指纹图谱中共有峰进行指认。结果得到分离度和重复性良好的GFC三萜类成分指纹图谱,确定了20个共有峰,其中1~7、10、12、14~17号峰共13个共有峰来自于茯苓,8、11号峰来自于桂枝,9号峰来自于白芍和牡丹皮,13号峰来自于桃仁、白芍、牡丹皮和桂枝。10批成品指纹图谱相似度在0.90以上。UPLC-Q-TOF/MS共鉴定出15个成分,分别为常春藤皂苷(1)、去氢土莫酸(2)、土莫酸(3)、猪苓酸C(4)、3-表去氢土莫酸(6)、茯苓酸D(7)、α-亚麻酸(9)、去氢茯苓酸(10)、齐墩果酸(11)、茯苓酸(12)、亚油酸(13)、棕榈油酸甲酯(15)、棕榈酸(16)、棕榈酸乙酯(17)、胡萝卜苷(18)。结论建立的UPLC指纹图谱有较好的精密度、重复性和稳定性,适用于GFC的质量控制。
OBJECTIVE: To establish a UPLC fingerprinting method for triterpene constituents of Guifu Fuling capsule (GFC), and to provide a new method for evaluating the quality of GFC. Methods The column was eluted with acetonitrile-0.1% phosphoric acid aqueous solution with a mobile phase of Agilent Zorbox Eclipse Plus HD C18 (100 mm × 2.1 mm, 1.8 μm) with gradient elution at a flow rate of 0.2 mL / The wavelength is 210 nm. The common peaks in fingerprints were identified by Q-TOF / MS. Results The fingerprints of GFC triterpenoids with good resolution and reproducibility were obtained and 20 common peaks were identified. Among them, 13 common peaks of 1 ~ 7, 10, 12 and 14 ~ 17 were from Poria, 8,11 No. peak from Guizhi, peak No. 9 from peony and moutan, peak No. 13 from peach kernel, white peony root, peony bark and cassia twig. 10 batches of fingerprints similarity of 0.90 or more. A total of 15 components were identified by UPLC-Q-TOF / MS, including Ivy saponin (1), Dehydroartemoformate (2), Trimellitic acid (3), Polyporus umbellate C (4) (7), α-linolenic acid (9), hydrogenated palmitic acid (10), oleanolic acid (11), pachyrin acid (12), linoleic acid 13), methyl palmitate (15), palmitic acid (16), palmitic acid ethyl ester (17) and daucosterol (18). Conclusion The established UPLC fingerprinting has good precision, repeatability and stability and is suitable for the quality control of GFC.