摘要
目的建立一种适合同时测定平卧菊三七Gynura procumbens水提物中9种主要有效成分(芹菜素、槲皮素、芦丁、杨梅素、绿原酸、原儿茶酸、对香豆酸、咖啡酸、山柰酚)的HPLC-MS/MS方法。方法 40 mg平卧菊三七水提物经甲醇(每次4 m L)超声提取2次,合并提取液并定容到10 m L。色谱分离采用Shim-pack ODS C18(150 mm×2.0 mm,4.6μm)分离柱,甲醇-0.1%甲酸水溶液为流动相,梯度洗脱,体积流量0.2 m L/min。质谱检测采用负离子多反应监测模式,并以和厚朴酚为内标。结果所测9种主要有效成分在测定质量浓度范围内线性关系良好,r均大于0.999 5;精密度、重复性和稳定性良好;平均加样回收率为91.0%~101.3%,RSD≤3.31%。结论建立的HPLC-MS/MS方法用于同时测定平卧菊三七水提物中9种主要有效成分,灵敏度高、专属性好。
Objective To develop a high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS） method for simultaneous determination of nine components（apigenin, quercetin, rutin, myricetin, chlorogenic acid, protocatechuate acid, p-coumaric acid, caffeic acid, and kaempferol） in Gynura procumbens aqueous extract. Methods Gynura procumbens aqueous extract（40 mg） was pretreated by two-step ultrasonic extraction using methanol（4 m L each time） as solvent and dissolved to 10 m L. Chromatographic separation was performed on Shim-pack ODS C18 column（150 mm × 2.0 mm, 4.6 μm） at a flow rate of 0.2 m L/min by a gradient elution, using methanol-0.1% formic acid water solution as mobile phase. The MS detection for the nine tested components was performed in negative ion multiple reaction monitoring mode using honokiol as an internal standard（IS）. Results All of the analytes showed good linearity（r ≥ 0.999 4） in the tested ranges. The precision, repeatability, and stability of the method were good for the nine components. The average recoveries were in the range of 91.0%—101.3%（RSD ≤ 3.31%）. Conclusion The established HPLC-MS-MS method has been proven to be highly sensitive and effective for simultaneous determination of the nine testing components in G. procumbens aqueous extract.
出处
《中草药》
CAS
CSCD
北大核心
2017年第2期294-298,共5页
Chinese Traditional and Herbal Drugs
基金
湖北省自然科学基金重点项目(2013CFA067)
