[目的]建立QuEChERS-超高效液相色谱-串联质谱法同时检测苦荞样品中10种真菌毒素。[方法]苦荞样品经水和乙腈提取后,采用QuEChERS方法净化。通过超高效液相色谱-三重四级杆质谱在多反应监测模式(MRM)下进行目标真菌毒素的分析。试验对样品前处理、仪器分析条件进行优化;考察方法的基质效应、检出限、精密度、回收率等参数。[结果]根据基质效应考察结果,50%的目标真菌毒素具有显著的信号抑制/增强效应。为了补偿基质效应的影响,选用基质配标法进行目标真菌毒素的分析。方法的线性范围为0.5~50.0μg/L(对于黄曲霉毒素B 2、G 2,线性范围为0.125~12.500μg/L),检出限和定量限分别低至0.011和0.040μg/L,回收率为89.70%~105.83%,RSD<9%(n=6)。[结论]建立的方法简便、可靠,具有较好的灵敏度和准确性,能有效用于苦荞样品中多组分真菌毒素的检测。
[Objective]To establish an analysis method for simultaneous determination of 10 mycotoxins in buckwheat samples based on QuEChERS-ultra-high performance liquid chromatography-tandem mass spectrometry.[Method]As a typical run,mycotoxins were extracted with water and acetonitrile,followed by purification with QuEChERS procedure.The target mycotoxins were analyzed by UPLC-MS/MS in multiple reaction monitoring(MRM)mode.The sample pretreatment and instrumental analysis method were respectively optimized.Finally,matrix effect,detection limits,precision and accuracy were investigated.[Result]According to the investigation of matrix effect,50%of the target mycotoxins have encountered prominent signal suppression/enhancement.To compensate the significant matrix effect,matrix-matched calibration curves were finally employed in this study.The linear range of targets were 0.5-50.0μg/L(0.125-12.500μg/L for AFB2,AFG2).Detection limits(LOD)and quantification limits(LOQ)were respectively detected down to 0.011 and 0.040μg/L.Recoveries were obtained ranging from 89.70%to 105.83%with RSD<9%.[Conclusion]The established method exhibits several advantages of simplicity,reliability,good sensitivity and accuracy.It is feasible and effective to apply this method for determination of multi-mycotoxins in buckwheat samples.
Journal of Anhui Agricultural Sciences