TY - JOUR
T1 - Determination of deoxynivalenol (vomitoxin) by high-performance liquid chromatography with electrochemical detection
AU - Sylvia, Victor L.
AU - Phillips, Timothy D.
AU - Clement, Beverly A.
AU - Green, Justin L.
AU - Kubena, Leon F.
AU - Heidelbaugh, Norman D.
PY - 1986
Y1 - 1986
N2 - A rapid method for the analysis of deoxynivalenol (DON) was developed using high-performance liquid chromatography (HPLC) with reductive electrochemical detection (ED). Deoxynivalenol produced by Fusarium roseum growing on solid cornmeal and rice substrates and from naturally contaminated wheat was extracted and quantitated via ED. DON levels in wheat were verified by gas chromatography and structurally confirmed by mass spectrometry. DON was optimally resolved by HPLC employing a radially compressed octadecylsilane column and a mobile phase of deoxygenated methanol-40 mM borate buffer (35:65) at a flow-rate of 1.0 ml/min. Under these conditions DON exhibited an average retention time of 3.6 min. Reductive ED (-1.4 V) allowed a 12-fold increase in sensitivity and greater selectivity than classical UV absorption at 224 nm. A detection limit for DON of 25 pg/ μl was achieved under these conditions. The determination of DON in crude grain extracts was hindered by extractable interfering substances, whereas ED was more functional-group selective (i.e. reduction of the carbonyl moiety). ED permits a direct quantitation of DON from crude grain extracts and may facilitate the determination of this agent and associated metabolites in biological samples.
AB - A rapid method for the analysis of deoxynivalenol (DON) was developed using high-performance liquid chromatography (HPLC) with reductive electrochemical detection (ED). Deoxynivalenol produced by Fusarium roseum growing on solid cornmeal and rice substrates and from naturally contaminated wheat was extracted and quantitated via ED. DON levels in wheat were verified by gas chromatography and structurally confirmed by mass spectrometry. DON was optimally resolved by HPLC employing a radially compressed octadecylsilane column and a mobile phase of deoxygenated methanol-40 mM borate buffer (35:65) at a flow-rate of 1.0 ml/min. Under these conditions DON exhibited an average retention time of 3.6 min. Reductive ED (-1.4 V) allowed a 12-fold increase in sensitivity and greater selectivity than classical UV absorption at 224 nm. A detection limit for DON of 25 pg/ μl was achieved under these conditions. The determination of DON in crude grain extracts was hindered by extractable interfering substances, whereas ED was more functional-group selective (i.e. reduction of the carbonyl moiety). ED permits a direct quantitation of DON from crude grain extracts and may facilitate the determination of this agent and associated metabolites in biological samples.
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U2 - 10.1016/S0021-9673(01)86953-3
DO - 10.1016/S0021-9673(01)86953-3
M3 - Article
C2 - 3745365
AN - SCOPUS:0022508662
VL - 362
SP - 79
EP - 85
JO - Journal of Chromatography A
JF - Journal of Chromatography A
SN - 0021-9673
IS - C
ER -