超高效液相色谱-串联质谱法测定食品中黄曲霉毒素B1和M1的方法研究

应用超高效液相色谱-串联质谱联用技术（UPLC-MS/MS）,在多反应离子检测（MRM）方式下对食品中的黄曲霉毒素B1（AFB1）和M1（AFM1）污染量进行检测.样品经乙腈-水混合试剂提取,中性氧化铝柱净化,经Agilem ZORBAX Eclipse plus C18色谱柱（100 mm×4.6 mm,1.8 μm）,以甲醇和10 mmol/L NH4Ac溶液（含0.1％的甲酸）为流动相洗脱分离,以MRM方式进行定量分析.AFB1和AFM1分别在0.12～6.12 μg/L和0.11～2.28 μg/L质量浓度范围内线性关系良好,相对标准偏差（RSD）＜5％,加标回收率为81.3％～97.2％.该方法具有低成本、准确、快速、简便、灵敏度高等优点,可满足我国对AFB1和AFM1检测限要求.

Determination of aflatoxins B1 and M1 in food by UPLC-MS/MS

A method was established to determine aflatoxin B1 （AFB1） and M1 （AFM1） in food by UPLC-MS/MS.This research focused on the detection ofAFB1 and AFM1 in food under multiple reaction monitoring （MRM） mode.Sample was extracted by acetonitrile aqueous solution,cleaned up with neutral alumina column.The analysis was performed on Agilent ZORBAX Eclipse plus C18 column （100 mn×4.6 mm,1.8 μm）,using methanol and 10 mmol/L NH4Ac solution （containing formic acid 0.1％） as mobile phase elution separation,quantitative analysis by MRM.The calibration curves were in good linear relationship in the range of 0.12-6.12 μg/L for AFB1 and 0.11-2.28 μg/L for AFM1.The relative standard deviation was less than 5％,and the adding standard recovery was in the range of 81.3％-97.2％.This method has advantages of low cost,accurate,rapid,simple and high sensitivity,which can meet the detection limit to AFB1 and AFM1 in China.