新疆市售小麦粉中脱氧雪腐镰刀菌烯醇的污染水平调查

Contamination survey of the Deoxynivalenols in wheat flour from in the market of Xinjiang

目的建立超高效液相色谱-串联质谱法(UPLC-MS/MS)检测面粉中脱氧雪腐镰刀菌烯醇的方法,并了解新疆市售小麦粉中脱氧雪腐镰刀菌烯醇的污染状况。方法采用负离子多反应监测模式,以^(13)C-DON为内标,样品用乙腈-水(86∶14,V/V)萃取后再用Mycosep TM 226净化柱净化。同时对新疆部分地州超市和农贸市场销售的84份小麦粉中DON、3-ADON、15-ADON的含量进行测定,数据结果采用GB 2761—2011《食品中真菌毒素限量》中规定的限量值,评价小麦粉中脱氧雪腐镰刀菌烯醇的污染水平。结果 3种毒素的浓度为0.5 ng/ml^500 ng/ml时,线性关系良好,相关系数(r)均>0.990。在抽检的84份小麦粉中,3-ADON均未检出,DON与15-ADON的检出率分别为51.2%、28.6%,DON与15-ADON的联合污染率为22.6%。结论该方法适用于小麦粉中脱氧雪腐镰刀菌烯醇的检测,新疆市售小麦粉中存在脱氧雪腐镰刀菌烯醇的污染状况。

Objective A ultra performance liquid chromatography- tandem mass spectrometric（ UPLC- MS/MS） method was developed for the determination of Deoxynivalenols in wheat flour,and investigate Deoxynivalenol contamination status in wheat flour from markets in Xinjiang. Methods The negative ion multiple reaction monitoring mode was used,and-（13）C- DON was used as internal standard. The sample was extracted with acetonitrile- water（ 86∶14,V/V）,then sample purification were performed on Mycosep TM 226 column. At the same time on the content of DON,3- ADON and 15- ADON of 84 wheat flour in Xinjiang supermarkets and farmers market were determined,then wheat flour deoxynivalenol contamination levels were assessed according to the prescribed limits in GB 2761—2011 Mycotoxins Limitation in Food. Results When the concentration of 3kinds of toxin was 0. 5 ng/ml- 500 ng/ml,the linear relationship was good,and correlation coefficient（ r） were all 0. 990.In the sampling of 84 wheat flour,3- ADON were not detected; the detection rates of DON and 15- ADON were 51. 2% and28. 6% respectively,and the combined pollution rate of DON and 15- ADON was 22. 6%. Conclusion This method is suitable for the detection of Deoxynivalenol in wheat flour,and the pollution of Deoxynivalenol was existed in wheat flour of Xinjiang.