摘要
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 the UPLC fingerprint oftriterpenoids in Guizhi Fuling Capsule （GFC） and give a new method for quality control. Methods UPLC was used on an Agilent Zorbox Eclipse Plus HD C18 （100 mm × 2.1 mm, 1.8 μm） column with the gradient elution solvent system composed of acetonitrile-0.1% H3PO4 water solution as mobile phase, the flow rate was 0.2 mL/min, the column temperature was 30 ℃, and the detection wavelength was 210 nm. The common peaks were identified by Q-TOF/MS. Results The UPLC fingerprints oftriterpenoids in GFC were established. Totally 20 common peaks were selected as the fingerprint peaks of GFC, of which a total of 13 mutual peaks （1-7, 10, 12, and 14-17） fromPoria, the peaks of number 8 and 11 were from Cinnamomi Ramulus, the peak of number 9 was from Paeoniae Radix Alba and Moutan Cortex, and the peak of number 13 was from Persicae Semen, Paeoniae Radix AIba, Moutan Cortex, and Cinnamomi Ramulus. The sinailarity among the fingerprint of 10 batches of GFC samples were 0.90. Fifteen chemical components were identified by UPLC-Q-TOF/MS, which were 1-hederagenin, 2-dehydrotumulosic acid, 3-tumulosil acid, 4-polyporenic acid C, 6-3-epidehydrotumulosic acid, 7-poricoic acid D, 9-α-linolenic acid, 10-dehydropachymic acid, 11-oleanolic acid, 12-pachymic acid, 13-1inolic acid, 15-methylcis-9-hexadecenoate, 16-palmitic acid, 17-palmitic acid ethyl ester, and 18-daucosterol. Conclusion The established UPLC fingerprint has desirable precision,reproducibility, and stability, and could be applied to the quality control of GFC.
出处
《中草药》
CAS
CSCD
北大核心
2016年第16期2857-2862,共6页
Chinese Traditional and Herbal Drugs
基金
科技部重大新药创制项目(2013ZX09402203)
