QuEChERS结合高效液相色谱-串联质谱法测定粮谷中16种真菌毒素

Simultaneous Determination of 16 Mycotoxins in Grains by QuEChERS and HPLC-MS/MS

建立了QuEChERS结合高效液相色谱-串联质谱仪(HPLC-MS/MS)同时测定粮谷中16种真菌毒素残留量的方法,样品经乙腈-水-乙酸(84∶15∶1,v/v)溶液超声提取,提取液采用C18、MgSO4净化,净化液过0.22μm微孔滤膜,用HPLC-MS/MS分析检测。Acquity UPLC BEH C18柱为分析柱,甲醇/乙腈(4+6)-0.1%甲酸水溶液为流动相进行梯度洗脱,采用电喷雾正负离子(ESI+、ESI-)模式同时电离,多反应监测(MRM)模式检测,外标法定量。结果表明,16种真菌在相应的浓度范围内线性关系良好(相关系数r2>0.995),方法定量限为0.3~3.5μg/kg,在低、中、高3个不同浓度的添加水平下,平均回收率为90.6%~106.5%,相对标准偏差≤8.8%(n=6),满足日常检测要求。该方法前处理简单,测定快速、准确,灵敏度高,适用于粮谷中16种真菌毒素残留的定性和定量分析。

A method of HPLC-MS/MS coupled with QuEChERS-based extraction had been developed for simultaneous determination of 16 mycotoxins in grains as follows:the samples were extracted by ultrasonic with acetonitrile-water-acetic acid(84∶15∶1,v/v)solution,and purified by C18 and MgSO4 sorbents,then filtered through 0.22μm microporous membrane,and finally detected by HPLCMS/MS.The LC separation was performed on Shimadzu LC-20ADXR system with a BEH C18 column with methanol/acetonitrile(4∶6)and 0.1%formic acid aqueous solution as the mobile phase for gradient elution.After LC separation,MS/MS was adopted for multiple reaction monitoring(MRM)in positive and negative mode.The correlation coefficients of linear calibration curves were above 0.995 in the corresponding concentration ranges.The limits of detection(LODs)were between 0.3μg/kg and 3.5μg/kg.The average recoveries of the 16 mycotoxins ranged from 90.6%to 106.5%,and the relative standard deviations(RSD)were lower than 8.8%in spiked sample at three levels.The results indicated that this method was fast,easy,sensitive,and suitable for the qualitative and quantitative analysis of the 16 mycotoxins in grains.