超高效液相色谱-串联质谱法快速测定小麦中黄曲霉毒素B_(1)

The Rapid Detection of Aflatoxin B_(1) in Wheat by UPLC-MS/MS

基于GB 5009.22—2016第一法,建立小麦中黄曲霉毒素B_(1)的超高效液相色谱串联三重四极杆质谱法(UPLC-MS/MS法)。小麦样品经粉碎、提取和直接稀释,采用C_(18)柱进行色谱分离,以4.0 mmol/L乙酸铵溶液(A)—甲醇(B)为流动相,梯度洗脱。用电喷雾正离子多反应监测模式(MRM)扫描。研究结果表明,建立的UPLC-MS/MS法在0.1~10.0 ng/mL范围内具有良好的线性关系,其相关系数R^(2)为0.9997;检出限(LOD)为0.004μg/kg,定量限(LOQ)为0.01μg/kg;相对标准偏差(RSD)为0.30%~11.50%;加标回收率为91.7%~100.9%。该方法操作简单,灵敏度高,成本低,可满足实验室快速、准确定量分析大批量小麦中黄曲霉毒素B_(1)的检测需求。

Based on the first method of GB 5009.22—2016,establishing a method for the determination of aflatoxin B_(1) in wheat by an ultra-high performance liquid chromatography with triple quadrupole mass spectrometry(UPLC-MS/MS).samples are crushed,extracted and directly diluted.the aflatoxin B_(1) diluent was separated by a C_(18) column and the mobile phase consisted of 4.0 mmol/L ammonium acetate-methanol under gradient eluting.Multiple-reaction monitoring(MRM)was performed to identify and quantify aflatoxin B_(1).The results of research shows good linearities(0.1-10.0 ng/mL)for aflatoxin B_(1) in the certain correlation ranges with the coefficients of 0.9997.The limit of detection(LOD)was 0.004μg/kg and the limit of quantification(LOQ)was 0.01μg/kg.The relative standard deviations ranged from 0.30%to 11.50%.The average recoveries ranged from 91.7%to 100.9%.The UPLC-MS/MS method is simple,sensitive,fast,and low in cost,which can meet the requirements of laboratory for rapid and accurate quantitative analysis of aflatoxin B_(1) in wheat.