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巴西南部小麦粉中脱氧雪腐镰刀菌烯醇的TLC定量方法评估及存在情况

Evaluation of the TLC quantification method and occurrence of deoxynivalenol in wheat flour of southern Brazil.

作者信息

Rocha Denise Felippin de Lima, Oliveira Melissa Dos Santos, Furlong Eliana Badiale, Junges Alexander, Paroul Natalia, Valduga Eunice, Backes Geciane Toniazzo, Zeni Jamile, Cansian Rogério Luis

机构信息

a Department of Food Technologyb Department of Chemistry and Foodc Department of Food Engineering , IFFarroupilha Campus Santo Augusto , Santo Augusto , Brazil.

b Department of Chemistry and Food , Universidade Federal de Rio Grande (FURG) , Rio Grande , Brazil.

出版信息

Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2017 Dec;34(12):2220-2229. doi: 10.1080/19440049.2017.1364872. Epub 2017 Sep 7.

Abstract

The study evaluated a QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) extraction method for use with a TLC quantification procedure for deoxynivalenol (DON). It also surveyed DON occurrence in wheat flour from the southern region of Brazil. Forty-eight wheat flour samples were analysed, divided into 2 different harvest lots, each consisting of 24 different brands. The detection and quantification limits of the method were 30 and 100 ng of DON on the TLC plate. The various concentrations of DON presented high linearity (R = 0.99). A negative matrix effect (-28%) of the wheat flour was verified, with suppression of the chromatographic signal of DON, and 80.2-105.4% recovery. The TLC method was reliable for DON evaluation, with a coefficient of variation of less than 10%. High-performance liquid chromatography of lot 2 samples confirmed the presence of DON in all samples identified DON-positive by the TLC technique. Of the 48 wheat flour samples in lots 1 and 2 analysed by TLC, 33.3 and 45.8% of the samples respectively were above the Brazilian legislation limit. Correlations were observed between the water activity and DON content, and between the fungal count and moisture content of the wheat flours.

摘要

该研究评估了一种用于脱氧雪腐镰刀菌烯醇(DON)薄层色谱定量分析程序的QuEChERS(快速、简便、廉价、高效、耐用且安全)提取方法。研究还调查了巴西南部地区小麦粉中DON的存在情况。共分析了48个小麦粉样品,分为2个不同的收获批次,每个批次包含24个不同品牌。该方法在薄层板上对DON的检测限和定量限分别为30 ng和100 ng。不同浓度的DON呈现出高度线性(R = 0.99)。证实了小麦粉存在负基质效应(-28%),即抑制了DON的色谱信号,回收率为80.2 - 105.4%。薄层色谱法对于DON评估是可靠的,变异系数小于10%。对第2批次样品的高效液相色谱分析证实,通过薄层色谱技术鉴定为DON阳性的所有样品中均存在DON。通过薄层色谱分析的第1批次和第2批次的48个小麦粉样品中,分别有33.3%和45.8%的样品超过了巴西法规限值。观察到小麦粉的水分活度与DON含量之间,以及真菌计数与水分含量之间存在相关性。

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