多功能净化柱净化-超高液相色谱串联质谱法检测云南所售部分面条及面条制品中的6种真菌毒素

Determination of 6 fungal toxins in some noodles and noodle products in Yunnan province by multifunctional purification column purification-ultra performance liquid chromatography tandem mass spectrometry

目的建立多功能净化柱净化-超高液相色谱-串联质谱法检测云南所售部分面条及面条制品中脱氧雪腐镰刀菌烯醇、3-乙酰脱氧雪腐镰刀菌烯醇、15-乙酰脱氧雪腐镰刀菌烯醇、雪腐镰刀菌烯醇、赭曲霉毒素A和玉米赤霉烯酮6种真菌毒素的含量。方法样品经乙腈-水-甲酸(70:29:1,F:F:F)溶液浸泡提取,通过Pribo Fast®M226多功能净化柱净化,采用超高液相色谱-串联质谱的多反应监测模式进行分析,外标法进行定量。结果6种真菌毒素在0.05~400 ng/L范围内线性关系良好(r>0.994),加标回收率为87.6%~10丨.3%,相对标准偏差为1.09%~3.65%。81份面条样品中,脱氧雪腐镰刀菌烯醇检出含量为15.2~664 ng/kg,检出率为98.77%,检测值均未超过国家食品安全标准规定的参考限量值,其余5种真菌毒素均为未检出。结论本检测方法具有快速便捷、准确性好、灵敏度高、特异性强等特点,适用于面条中6种真菌毒素的同时测定。

Objective To establish a method for determination of deoxynivalenol, 3-acetyl deoxynivalenol,15-acetyl deoxynivalenol, flisarium oxysporum, ochratoxin A and zearalenone in some noodles and noodle productssold in Yunnan province by multifunctional purification column purification-ultra performance liquidchromatography tandem mass spectrometry. M ethods The sample was extracted by soaking in acetonitrile formicacid water (70:29:1, V: V: V) , purified by Pribo Fast®M226 multi-purification column, and analyzed by ultra-highliquid chromatography-tandem mass spectrometry with multiple reaction monitoring mode, and quantificativelyanalyzed by external standard method. R esults The 6 fungal toxins had good linear relationships in the range of 0.05-400 |ig/L(r>0.994). The recoveries were 87.6%-101.3%, with the relative standard deviations of 1.09%-3.65%.Among the 81 noodle samples, the detection content of deoxynivalenol was 15.2〜664 (ig/kg, and the detection ratewas 98.77%. The detection values did not exceed the reference limit value specified by the national food safetystandards, and the other 5 fungi toxins were not detected. Conclusion This method has the characteristics of fast,convenient, accurate, high sensitivity and strong specificity. It is suitable for simultaneous determination of 6 kinds offungal toxins in noodles.