Purification of cyclopiazonic acid by liquid chromatography.
A purification procedure for cyclopiazonic acid has been developed, using sequential preparative and semi-preparative liquid chromatography. Crude cyclopiazonic acid (324 mg) was extracted from a 1 L fermentation medium with chloroform-methanol (80 + 20), dried, dissolved in chloroform, and chromatographed on an oxalic acid/silica preparative column with chloroform-methanol (99 + 1) as the eluant. A semi-preparative oxalic acid/silica column and chloroform-methanol (99.5 + 0.5) were then used for rechromatography of the partially purified cyclopiazonic acid. This second chromatographic treatment yielded fractions from which cyclopiazonic acid was readily crystallized (106.7 mg; 33% recovery). Analytical chromatography was developed using an amino column in an ion-exchange mode, with a methanol-phosphate buffer eluant. Response was linear from 10 to 800 micrograms/injection of standard solutions. Cyclopiazonic acid chemically binds sodium from soda-lime vials.
Peterson
R E
RE
U.S. Department of Agriculture, Northern Regional Research Center, Peoria, IL 61604.
Shannon
G M
GM
Shotwell
O L
OL
D002851:Chromatography, High Pressure Liquid; D007211:Indoles / Q000302:isolation & purification*; D013058:Mass Spectrometry; D009183:Mycotoxins / Q000302:isolation & purification*
D007211:Indoles; D009183:Mycotoxins; C000543:cyclopiazonic acid