基于UPLC-MS-MS技术快速测定花生中4种黄曲霉毒素

摘要

建立了花生中4种黄曲霉毒素的超高液相色谱-三重四极杆串联质谱(UPLC-MS-MS)检测的方法.样品经80%乙腈-水溶液振荡超声提取后,采用多功能净化柱净化.待测物经Kinetex SB-C18色谱柱分离,甲醇-0.1%甲酸溶液为流动相,梯度洗脱,三重四级杆串联质谱多反应离子监测(MRM)方式检测,外标法定量.结果表明:4种黄曲霉毒素在各自的线性响应范围内线性关系良好,相关系数均大于0.999,方法的检出限为0.014~0.025 μg/kg,空白样品中加标回收率为72.25% ~89.46%,RSD在4.01% ~9.56%之间.该方法前处理简单快速、净化效果好、检出限低,适合花生中多种黄曲霉毒素的同时快速测定.%A UPLC - MS - MS method for detecting four kinds of aflatoxins in peanut was established.The samples were extracted in 80% acetonitrile - water solution by ultrasonic vibration, and purifiedusing a multi - functional cleanup column. The sample was separated by Kinetex SB - C18 chromatographiccolumn, subjected to gradient elution using methanol - 0. 1% formic acid solution as the mobilephase, then detected by triple - quadrupole mass spectrometry with multiple reaction monitoring(MRM), and analyzed quantitatively by the external standard method. The results suggested that fourkinds of aflatoxins presented good linearity within their respectively linear response ranges, and the coefficientof correlation were above 0. 999; the method's limit of detection was 0. 014 -0. 025 μg/ kg; the recoveriesof standard addition for blank samples were 72. 25% - 89. 46% with the RSDs 4. 01% -9. 56%. Characterized by simple and quick pre - treatment, good purification effect, and low limit of detection,this method could be used for simultaneously rapid determination of various aflatoxins in peanut.