超高液相色谱串联质谱法测定小麦粉中真菌毒素

Determination of Mycotoxins in Wheat Flour by UPLC-MS/MS

建立小麦粉中雪腐镰刀菌烯醇(NIV)、隐蔽型脱氧雪腐镰刀烯醇(Deepoxy-DON)、脱氧雪腐镰刀菌烯醇(DON)及衍生物(3A-DON、15A-DON)、玉米赤霉烯酮(ZEN)常见6种真菌毒素的同时测定方法。试样用多功能净化柱净化,液相色谱-串联质谱基质内标法定量测定。结果表明6种真菌毒素的检出限在0.50μg/kg^1.00μg/kg之间,线性相关系数R^2>0.994,3个水平加标回收率为82.1%~108.9%,RSD为4.6%~14.5%。采用本方法参加面粉中脱氧雪腐镰刀烯醇能力验证样品质控考核,统计结果 Z为-1.93,结果评价为满意。该方法准确、灵敏、高效,可适用于小麦粉中6种常见真菌毒素的定量分析。

The method to simultaneously determinate six kinds of common mycotoxins, included nivalenol （ NIV ）, deoxynivalenol concealed （Deepoxy-DON）, deoxynivalenol （DON）, deoxynivalenol derivatives （ 3A- DON, 15A- DON） and zearalenone（ZEN ） in wheat flour was established. The samples were purified with mul- tifunctional purifying column, then determinated by liquid chromatography tandem mass spectrometry with internal standard method. The results showed detection limits of six kinds mycotoxin were between 0.50 μg/kg and 1.00 μg/kg, the linear correlation coefficient R2 〉 0.994, three levels recovery were 82.1%-108.9 %, RSD were 4.6 %-14.5 %. The method used to ability verification and quality control assessment of deoxynivalenol in wheat flour, statistical results Z score was -1.93, the result was evaluated as satisfactory. The method is accurate, sensitive and efficient and applicable to quantitative analysis of six kinds of common mycotoxin in wheat flour.