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薄层色谱法测定加工谷物产品中的脱氧雪腐镰刀菌烯醇

Thin layer chromatographic determination of deoxynivalenol in processed grain products.

作者信息

Trucksess M W, Flood M T, Page S W

出版信息

J Assoc Off Anal Chem. 1986 Jan-Feb;69(1):35-6.

PMID:3949696
Abstract

The thin layer chromatographic (TLC) method of Trucksess et al. (J. Assoc. Off. Anal. Chem. (1984) 67, 40-43) was modified for the determination of deoxynivalenol (DON) in high-sugar breakfast cereals, corn syrup, and beer. Celite was added to the substrate before extraction with acetonitrile-water (84 + 16). After filtration through an alumina-charcoal-Celite (0.5 + 0.7 + 0.3) column, the filtrate was evaporated to dryness and redissolved in water, which was passed through an octylsilyl reverse phase column. DON was eluted with anhydrous ethyl ether. The residue remaining after the eluate was evaporated to dryness was dissolved in CHCl3-acetonitrile (4 + 1) and chromatographed on AlCl3-impregnated silica gel TLC plates. The blue fluorescent DON spot was quantitated fluorodensitometrically after the TLC plate was heated at 120 degrees C for 7 min. Recoveries of DON added to breakfast cereals at 100, 200, and 400 ng/g levels and to syrup and beer at 50, 100, and 200 ng/g levels averaged 86%. The limit of determination in these products was about 50 ng/g.

摘要

对Trucksess等人(《美国官方分析化学师协会杂志》(1984年)67卷,40 - 43页)的薄层色谱(TLC)方法进行了改进,用于测定高糖早餐谷物、玉米糖浆和啤酒中的脱氧雪腐镰刀菌烯醇(DON)。在用乙腈 - 水(84 + 16)萃取之前,向底物中加入硅藻土。通过氧化铝 - 活性炭 - 硅藻土(0.5 + 0.7 + 0.3)柱过滤后,将滤液蒸发至干并重新溶解于水中,然后通过辛基甲硅烷基反相柱。用无水乙醚洗脱DON。将洗脱液蒸发至干后剩余的残渣溶解于氯仿 - 乙腈(4 + 1)中,并在浸渍有AlCl₃的硅胶TLC板上进行色谱分析。在将TLC板于120℃加热7分钟后,用荧光密度计对蓝色荧光的DON斑点进行定量。添加到早餐谷物中浓度为100、200和400 ng/g以及添加到糖浆和啤酒中浓度为50、100和200 ng/g的DON的回收率平均为86%。这些产品中的测定限约为50 ng/g。

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