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Countercurrent purification of the tetrahydro iso‐α acids derived from Humulus lupulus L.
Author(s) -
Dahlberg Clinton J.,
Traub James S.,
Tripp Matthew L.,
Bland Jeffrey S.,
Carroll Brian J.
Publication year - 2010
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.200900755
Subject(s) - humulus lupulus , chromatography , chemistry , solvent , hop (telecommunications) , countercurrent exchange , countercurrent chromatography , diastereomer , organic chemistry , column chromatography , computer network , physics , food science , pepper , computer science , thermodynamics
Recent biological research has shown that commercially available tetrahydro iso‐α acid (THIAA) extract exhibits a significant anti‐inflammatory response in cellular assays. To further elucidate the mechanism of the response, a method was developed and optimized for the purification of three THIAA cis congeners that are found in commercially available modified hop ( Humulus lupulus L.) extracts. Utilizing a Pharmatech Research hydrodynamic countercurrent separation instrument, the choice of solvent, pH and buffer composition were optimized to increase the overall efficiency. It was determined that a quaternary HEMWat (7:3:5:5, pH 5.3) solvent system is optimal for separating cis and trans diastereomers, whereas the binary solvent system of hexanes and aqueous buffer (1:1, pH 6.8) is optimal for the isolation of individual congeners. The optimal countercurrent separation method allows for sample loadings of 3 mg of sample per milliliter of column volume, minimal purification times (1–4 h) and greater than 90% homogeneity of individual THIAA congeners.