Supercritical fluid extraction of fumonisin B1 from grain dust.
Selim-MI; El-Sharkawy-SH; Popendorf-WJ
J Agric Food Chem 1996 Oct; 44(10):3224-3229
A supercritical fluid method for extracting fumonisin-B1 (116355830) (FB1) from grain dusts was developed. The procedure was intended for use with an online high performance liquid chromatography (HPLC) technique for determining FB1 in grain dust samples contaminated with Fusarium-moniliforme and was developed using spiked corn dust samples. Corn dust samples, 0.25 gram, were extracted with 15 milliliters (ml) of liquid supercritical carbon-dioxide in an SFX2- 10 system under a pressure of 1,200 pounds per square inch at 60 degrees-C for 20 minutes (min). Acetic-acid was added in the extraction cell and when the sample was added to the HPLC system. After the 20min extraction period, the supercritical carbon-dioxide was transferred to a collecting tube containing a 1:1 mixture of methanol/isooctane to trap the analyte. The methanol layer, containing the analyte, was evaporated to dryness. The residue was then reconstituted in 0.1 molar sodium-borate buffer (pH 8.5). After derivatization with fluorescamine solution, the sample was injected into an HPLC system fitted with an ultraviolet detector for analysis. Recovery experiments in which the supercritical extraction procedure was compared with the standard solvent/solvent extraction procedure using ethyl-acetate and a 3:1 mixture of methanol/water revealed that 40 times more FB1 could be recovered by supercritical fluid extraction than by solvent/solvent extraction. The FB1 detection limit using supercritical fluid extraction was estimated to be 150 parts per billion. Four replicate analyses of a naturally contaminated corn dust sample using supercritical fluid and solvent/solvent extraction found FB1 at concentrations of 78.16 and 2.12 parts per million (ppm), respectively. The corresponding relative standard deviations were 5.66 and 6.46%. The authors conclude that supercritical fluid extraction provides a fast, effective, and reproducible method for extracting FB1 from grain dust samples.
NIOSH-Publication; NIOSH-Grant; Grants-other; Mycotoxins; Analytical-methods; Fungi; Solvent-extraction; Grain-dusts; Chromatographic-analysis; Sample-preparation
Preventive Medicine and Environmental Health, University of Iowa ,137 Amrf Oakdale Campus, Iowa City, IA 52242
Journal of Agricultural and Food Chemistry
University of Iowa, Iowa City, Iowa