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Silver ion coordination countercurrent chromatography: Separation of β‐elemene from the volatile oil of Curcumae Rhizoma

Lu, Mengxia, Wang, Xiaoping, Bu, Zhisi, Lv, Liqiong, Tong, Shengqiang
Journal of separation science 2017 v.40 no.18 pp. 3740-3747
coordination compounds, countercurrent chromatography, gas chromatography-mass spectrometry, gel chromatography, oils, silver nitrate, solvents
In this work, the antitumor constituent β‐elemene was selectively separated from the volatile oil of the Curcumae Rhizoma by countercurrent chromatography with silver nitrate as selective reagent based on the formation of coordination complexes. A biphasic solvent system composed of n‐hexane/methanol/water (2:1.5:0.5, v/v/v) was selected, in which 0.15 mol/L of silver nitrate was added to the aqueous phase. The aqueous phase was used as the stationary phase for separation of β‐elemene by countercurrent chromatography after it was partially purified from the volatile oil by silica gel column chromatography. An enriched β‐elemene fraction was obtained by silica gel column chromatography to improve the percentage of β‐elemene from 16.5 to 46.1%. Subsequently, β‐elemene was further purified from 445 mg of the partially purified sample of volatile oil by countercurrent chromatography with silver nitrate as a selective reagent, yielding 145 mg of β‐elemene with greater than 99% purity, as determined by gas chromatography mass spectrometry. The recovery of β‐elemene from the crude volatile oil through two steps was around 63.6%.