小麦粉中2种新型真菌毒素含量测定方法

Determination Method of Two New Mycotoxins in Wheat Flour

建立固相萃取柱净化超高效液相色谱-串联质谱法测定小麦粉中白僵菌素和恩镰饱菌素B含量。样品中白僵菌素和恩镰饱菌素B采用酸化的乙腈-水溶液超声提取,PEP固相萃取柱净化后,采用超高效液相色谱-串联质谱进行检测。白僵菌素和恩镰饱菌素B分别在0~50 ng/mL和0~25 ng/mL质量浓度范围内具有良好线性关系,相关系数r值均大于0.999,在空白样品中添加白僵菌素(4.8,48和96μg/kg)和恩镰饱菌素B(2.4,24和48μg/kg)这3个浓度水平的2种真菌毒素标准品,平均回收率和相对标准偏差(n=6)分别在74.60%~99.31%和4.06%~8.10%之间,方法定量限分别为3μg/kg和1.5μg/kg,与QuEChERS快速净化方法相比,试验方法净化效果较好,基质抑制在可接受范围内。试验方法能准确、灵敏地检测小麦粉中白僵菌素和恩镰饱菌素B含量,可为了解小麦粉中2种新兴真菌毒素污染水平提供依据。

A method for determination of beauvericin and enniatin B in wheat flour by UPLC-MS/MS coupled with solid phase extraction column purification methods was to established.Beauvericin and enniatin B in wheat flour were ultrasonic extracted by acidified acetonitrile aqueous solution,purified through PEP solid phase extraction column and then determinate using UPLC-MS/MS.Beauvericin and enniatin B exhibited a good linear relationship at 0-50 ng/mL and 0-25 ng/mL respectively.The correlation coefficient r value of two mycotoxin were greater than 0.999.The average recovery and relative standard deviation(δRSD,n=6)were 74.60%-99.31%and 4.06%-8.10%under three levels of two mycotoxin standards were added in blank samples at concentration of beauvericin(4.8,48 and 96μg/kg)and enniatin B(2.4,24 and 48μg/kg).The quantitative limit of the method was 3μg/kg and 1.5μg/kg,respectively.Compared with QuEChERS method,the method had better purification effect and the matrix inhibition was within the acceptable range.The method was accurate and high in sensitive for the determination of beauvericin and enniatin B in wheat flour,and could provide a reference for assessing two mycotoxin contamination level beauvericin and enniatin B in wheat flour.