PMID- 12477199
OWN - NLM
STAT- MEDLINE
DCOM- 20030515
LR  - 20190729
IS  - 1060-3271 (Print)
IS  - 1060-3271 (Linking)
VI  - 85
IP  - 6
DP  - 2002 Nov-Dec
TI  - Determination of deoxynivalenol in whole wheat flour and wheat bran.
PG  - 1355-9
AB  - A liquid chromatographic (LC) method was developed for determining deoxynivalenol 
      (DON) in whole wheat flour and wheat bran. A 15 g test sample was extracted with 
      acetonitrile-water (84 + 16, v/v) and applied to a Romer MycoSep cleanup column. 
      The eluate was dried and then reconstituted in a 0.1 M phosphate buffer, pH 7.0, 
      and applied to a Vicam DONtest-LC cleanup column. The methanol eluate was 
      chromatographed with a methanol-water (17 + 83, v/v) mobile phase on a C18 column 
      with UV detection at 220 nm. Five replicates at each of 5 fortification levels 
      (0.25, 0.50, 1.0, 2.0, and 4.0 ppm), plus 5 controls, were determined for both 
      whole wheat flour and wheat bran. For flour, the average recoveries were 
      72.2-91.5% with relative standard deviations (RSDs) of 4.9-18.4%. The intra-assay 
      flour recovery was 82.4% with 9.8% RSD. A 5 replicate sample of naturally 
      incurred wheat had an average of 1.1 ppm DON with 6.7% RSD. For bran, average 
      recoveries of fortified samples were 69.5-99.7% with RSDs of 1.7-18.8%. The 
      intra-assay bran recovery was 81.5% with 8.9% RSD. The limit of detection (about 
      3x noise) for the method is 0.05 ppm; the correlation coefficient (linearity) was 
      >0.9995. The DON peak was clearly identified and easily integrated in the 
      chromatograms.
FAU - Rupp, Heidi S
AU  - Rupp HS
AD  - U.S. Food and Drug Administration, Pacific Regional Laboratory Northwest, 
      Bothell, WA 98021, USA. hrupp@ora.fda.gov
LA  - eng
PT  - Journal Article
PL  - England
TA  - J AOAC Int
JT  - Journal of AOAC International
JID - 9215446
RN  - 0 (Buffers)
RN  - 0 (Dietary Fiber)
RN  - 0 (Solutions)
RN  - 0 (Solvents)
RN  - 0 (Trichothecenes)
RN  - JT37HYP23V (deoxynivalenol)
SB  - IM
MH  - Buffers
MH  - Chromatography, Liquid
MH  - Dietary Fiber/analysis
MH  - Flour/*analysis
MH  - Mass Spectrometry
MH  - Reference Standards
MH  - Solutions
MH  - Solvents
MH  - Spectrophotometry, Ultraviolet
MH  - Trichothecenes/*analysis
MH  - Triticum/*chemistry
EDAT- 2002/12/13 04:00
MHDA- 2003/05/16 05:00
CRDT- 2002/12/13 04:00
PHST- 2002/12/13 04:00 [pubmed]
PHST- 2003/05/16 05:00 [medline]
PHST- 2002/12/13 04:00 [entrez]
PST - ppublish
SO  - J AOAC Int. 2002 Nov-Dec;85(6):1355-9.