期刊
SEPARATION AND PURIFICATION TECHNOLOGY
卷 260, 期 -, 页码 -出版社
ELSEVIER
DOI: 10.1016/j.seppur.2020.118208
关键词
Betulinic acid; Oleanolic acid; Triterpenoids; Triacontyl (C30); Simulated moving bed chromatography
资金
- Portuguese Foundation for Science and Technology/MCTES [UIDB/50011/2020, UIDP/50011/2020]
- Multibiorefinery project [POCI01-0145-FEDER-016403]
- Fundacao para Ciencia e a Tecnologia (Portugal) [SFRH/BD/126509/2016]
- FEDER funds through COMPETE2020 -Programa Operacional Competitividade e Internacionalizacao (POCI) [POCI-01-0145-FEDER-006939]
- Fundação para a Ciência e a Tecnologia [SFRH/BD/126509/2016] Funding Source: FCT
This study focused on the reversed-phase chromatographic separation of betulinic and oleanolic acids using a C30 stationary phase. The method of moments was used to determine the equilibrium constants and coefficients of the acids, which were validated by breakthrough curve modeling. The study also found that adding water to methanol/acetonitrile mixtures can efficiently precipitate the TTAs.
The reversed-phase chromatographic separation of two triterpenic acids (TTAs), betulinic and oleanolic acids, using a triacontyl (C30) stationary phase was addressed in this work. Methanol, water, acetonitrile, ethanol, isopropanol, ethyl acetate, acetone and mixtures thereof were tested, and the best mobile phase to conduct the separation was found to be methanol/acetonitrile 50/50 (%, v/v) at 23 degrees C, taking into account parameters like selectivity, resolution and TTAs solubility. The method of moments was used to determine the equilibrium constants of isotherms, the axial dispersion coefficients and the global linear driving force coefficients of pure betulinic and pure oleanolic acids. These parameters were then successfully validated by modeling unary and binary breakthrough curves. Simulated moving bed calculations showed that betulinic and oleanolic acids can be both obtained with purity of 99.2 % and productivity of 56.2 kg/(m(adsorbent)(3) day) using the packing material of an Acclaim C30 column with a 1-1-1-1 configuration with columns of 7.5 cm long. Finally, in order to recover the two TTAs from the SMB extract and raffinate streams, water was envisioned as a precipitation agent. Accordingly, the solubility of each TTA was measured in methanol/acetonitrile 70/30, 50/50, and 30/70 (%, v/v) modified with water. The obtained results showed that adding 65 % (%, v/v) of water it is possible to precipitate 98 % of the dissolved TTAs in all the tested methanol/acetonitrile mixtures.
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