Extraction and separation of pinosylvins by Centrifugal Partition Chromatography

Lorántfy, László; Kovács, Z.; Rutterschmidt, D; Misek, Z; Rajsch, G

doi:10.1055/s-0035-1565778

Cited by 1 publication

(1 citation statement)

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“…Considerations on Solvent Systems. Our previous experience with model molecules, 25 natural products, 26 and APIs 27 has shown that for most purification problems, a ternary system can provide good or satisfactory selectivity and loading capacity. It should also be mentioned, however, that quaternary solvent systems are more common in the lab-scale isolation of natural products than the ternary ones.…”

Section: Conceptmentioning

confidence: 99%

Continuous Industrial-Scale Centrifugal Partition Chromatography with Automatic Solvent System Handling: Concept and Instrumentation

Lorántfy

Rutterschmid

Örkényi

et al. 2020

Org. Process Res. Dev.

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Centrifugal partition chromatography (CPC) is an emerging separation technology in pharmaceutical and natural product purifications, reaching recently industrial-scale solutions. Because both the stationary and mobile phases are liquids in CPC, the solvent consumption of such separation processes is considered significant. Thus, automation is highly required in the preparation and recycling of the solvent mixtures for economical (i.e., continuous) CPC operation. Here, we report a feasible solution for this industrial issue, including the concept, algorithm, and instrumentation of solvent system handling. For majority of ternary solvent systems used in CPC separations, the linear correlation between the density and composition of the phases was recognized and utilized during the continuous solvent recycling. Hence, an efficient density-based composition adjustment algorithm was established in a mixer-settler unit using Coriolis flow meters for precise density monitoring of the upper and lower phases of the biphasic liquid system (BLS). In addition, a complete cascade consisting of a buffer, waste, a recycler (evaporator), and mixer-settler units was designed around the industrial-scale CPC device. The proof of concept was demonstrated by sequential industrial-scale CPC separations of a binary model mixture in the n-hexane/methanol/water (5/4/1, v/v/v) solvent system, followed by the purification of a crude steroid active pharmaceutical ingredient performed in the methyl isobutyl ketone/acetone/water (2/2/1, v/v/v) solvent system. The reproducibility of chromatographic performance and the productivity of the mixer-settler and evaporator units were satisfactory, enabling a robust and continuous operation of the developed separation process.

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Section: Conceptmentioning

confidence: 99%