Rupp Heidi S
U.S. Food and Drug Administration, Pacific Regional Laboratory Northwest, Bothell, WA 98021, USA.
J AOAC Int. 2002 Nov-Dec;85(6):1355-9.
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.
建立了一种液相色谱（LC）法测定全麦粉和麦麸中的脱氧雪腐镰刀菌烯醇（DON）。称取15 g测试样品，用乙腈-水（84 + 16，v/v）萃取，然后加到Romer MycoSep净化柱上。洗脱液经干燥后，再用pH 7.0的0.1 M磷酸盐缓冲液复溶，并加到Vicam DONtest-LC净化柱上。甲醇洗脱液用甲醇-水（17 + 83，v/v）流动相在C18柱上进行色谱分析，于220 nm处进行紫外检测。对全麦粉和麦麸分别在5个加标水平（0.25、0.50、1.0、2.0和4.0 ppm）下各进行5次重复测定，另加5个对照。对于面粉，平均回收率为72.2% - 91.5%，相对标准偏差（RSD）为4.9% - 18.4%。方法的批内面粉回收率为82.4%，RSD为9.8%。一份含天然DON的小麦重复5次测定的样品，平均DON含量为1.1 ppm，RSD为6.7%。对于麦麸，加标样品的平均回收率为69.5% - 99.7%，RSD为1.7% - 18.8%。方法的批内麦麸回收率为81.5%，RSD为8.9%。该方法的检测限（约为3倍噪声）为0.05 ppm；相关系数（线性）>0.9995。DON峰在色谱图中能清晰识别且易于积分。
