Zhang Xiaotian, Ji Feng, Li Yueqi, He Tian, Han Ya, Wang Daidong, Lin Zongtao, Chen Shizhong
School of Pharmaceutical Sciences, Peking University.
Analytical Center, Department of Analytical Instruments, Shimadzu (China) Co.
Anal Sci. 2018;34(4):407-413. doi: 10.2116/analsci.17P434.
In this study, an on-line supercritical fluid extraction (SFE) and supercritical fluid chromatography (SFC) method was developed for the rapid determination of oleanoic acid and ursolic acid in Chaenomelis Fructus. After optimization of the conditions, the two triterpenoid acids was obtained by SFE using 20% methanol as a modifier at 35°C in 8 min. They were resolved on a Shim-pack UC-X Diol column (4.6 × 150 mm, 3 μm) in 14 min (0 - 10 min, 5 - 10%; 10 - 14 min, 10% methanol in CO) with a backpressure of 15 MPa at 40°C. The on-line SFE-SFC method could be completed within 40 min (10.79 mg/g dry plant, R = 2.36), while the ultrasound-assisted extraction and HPLC method required at least 90 min (3.55 mg/g dry plant, R = 1.92). This on-line SFE-SFC method is powerful to simplify the pre-processing and quantitative analysis of natural products.
本研究建立了一种在线超临界流体萃取（SFE）和超临界流体色谱（SFC）法，用于快速测定木瓜中的齐墩果酸和熊果酸。条件优化后，以20%甲醇为改性剂，在35℃下经8分钟的SFE获得了这两种三萜酸。它们在Shim-pack UC-X二醇柱（4.6×150 mm，3μm）上于40℃、15 MPa背压下，在14分钟内实现分离（0 - 10分钟，5 - 10%；10 - 14分钟，CO中含10%甲醇）。在线SFE-SFC法可在40分钟内完成（干植物中含量为10.79 mg/g，R = 2.36），而超声辅助萃取和HPLC法至少需要90分钟（干植物中含量为3.55 mg/g，R = 1.92）。这种在线SFE-SFC法对于简化天然产物的预处理和定量分析具有强大作用。
