福建市售薏苡仁常见真菌毒素污染状况研究

Study on mycotoxins contamination status of coix seed in Fujian markets

目的建立同位素内标稀释超高效液相色谱-串联质谱(UPLC/MS/MS)快速测定真菌毒素的方法,了解福建市售薏苡仁中常见真菌毒素污染状况。方法粉碎均匀的薏苡仁经提取、离心、稀释后,加入同位素内标以校正基质干扰,用UPLC/MS/MS测定。用该法检测2015—2017年采自福建省农贸市场、超市等销售的薏苡仁50份。结果建立了同位素内标稀释UPLC/MS/MS快速测定真菌毒素残留的方法,本法灵敏度高、操作简单,可满足检测要求。50份薏苡仁16种常见真菌毒素污染情况分析结果,发现玉米赤霉烯酮和脱氧雪腐镰刀菌烯醇是主要的污染指标,检出率分别为34.0%和30.0%。参考GB 2761-2017规定,保质期内薏苡仁中玉米赤霉烯酮的超标率仅4%(2/50)。结论本研究所建立的同位素内标稀释超高效液相色谱-串联质谱(UPLC/MS/MS)法,测定快速、灵敏度高、操作简单,能满足真菌毒素的检测要求;应加强食品中真菌毒素污染情况监测,对消费量小的薏苡仁食品也需加强管理。

Objective To establish a rapid method for detecting mycotoxins by UPLC/MS/MS(Ultra high performance liquid chromatography tandem mass spectrometry)with isotopic internal standard dilution technique and to analyze the contamination status of mycrotoxins in coix seed in Fujian markets.Methods The coix seed flour was extracted,centrifugated and diluted,then isotope internal standard was added into the diluents to correct matrix interference and the diluents were detected by UPLC/MS/MS method.Totally 50 coix seeds collected from Fujian markets in 2015-2017 were detected with this method.Results A rapid method for detecting mycrotoxins residues in coix seed was established by using UPLC/MS/MS with isotopic internal standard dilution technique method.The established method is sensitive,simple and useful for detecting mycotoxins.The detection results of 16 kinds of common mycrotoxins residues in 50 coix seeds showed that deoxynivalenol and zearalenone were the main contamination indicators,the detection rates were 30%and 34%,respectively.Based on GB 2761-2017,the over standard rate of zearalenone residues in coix seeds was 4%(2/50)only in expiration date.Conclusion The established UPLC/MS/MS with isotopic internal standard dilution technique method is rapid,sensitive,simple and useful for testing of mycrotoxins.The monitoring of mycrotoxin contamination in food should be strengthened and the management of food with small consumption,sach as coix seed,should also be strengthened in the future.