食品中赭曲霉毒素A的前处理方法比较

The Comparative Study of Different Pretreatment Methods for Ochratoxin A in Food

为探究食品中霉菌产赭曲霉毒素A(OTA)精确、高效和经济的检测方法,将免疫亲和柱(IAC)、C18固相萃取柱(C18SPE)、液液萃取(LLE)、旋蒸浓缩(EC)和玻璃微纤维滤纸(GMF)相结合,采用液相色谱-四级杆静电场轨道阱质谱(LC-Q-Orbitrap)方法检测比较了4种前处理方法的差异性。结果表明,旋蒸浓缩联用玻璃微纤维滤纸(EC-GMF)的回收率显著高于其他组合,依次为EC-GMF(104.94%),IAC-GMF(92.76%),C18SPE-GMF(86.86%),LLE-GMF(55.42%);免疫亲和柱联用玻璃微纤维滤纸(IAC-GMF)的前处理净化效果最好,基底干净,杂质种类少且含量低。综合样品的检测效果和检测成本,旋蒸浓缩和玻璃微纤维滤纸相结合,以LC-Q-Orbitrap检测,可作为OTA检测的一种可行方法,该方法检出限为0.05 ng·m L-1,回收率为104.94%,相对标准偏差小于2.85%(n=4)。本研究可为食品中OTA检测提供理论参考。

To explore an accurate, efficient and economic detection method of Ochratoxin A （OTA） produced by molds in food, immune affinity column （IAC） , C18 solid phase extraction column （C18SPE） , evaporation concentration （EC） and liquid-liquid extraction （LLE） were selected to combine with glass microfiber filter （GMF） , respectively. The differences of four kinds of pretreatment methods for recovery of OTA in food with LC-Q-Orbitrap detection were investigated. Results showed that the recovery of EC-GMF is significantly higher than other combination methods, up to 104.94%, and followed IAC-GMF （92.76%）, C18SPE-GMF （86. 86% ） and LLE-GMF （55.42%）. The method of IAC-GMF showed the best effect because the basement is very clean. It is due to the less impure components and its lower content. An efficient method for OTA detection was established by LC-Q-Orhitrap analysis with a pretreatment of EC and GMF, considering the detection results and cost. The detection limit of this method was O. 05 ng· mL^-1, and its average recovery of standard addition in a positive sample reached 104.94% with a RSD less than 2.85% （n = 4）. The establishment of this method can provide reference for OTA detection in food.