二维液相色谱模拟柱后衍生系统检测粮食中黄曲霉毒素总量

Determination of Total Aflatoxin in Grain by Two-dimensional Liquid Chromatography Simulated Post-column Derivatization System

为建立一种由二维液相色谱模拟柱后衍生系统测定粮食中黄曲霉毒素B族G族总量的检测方法。以水68%+乙腈16%+甲醇16%为流动相,等度洗脱,流速:1.0 mL/min;柱温:40℃;进样体积:100μL;衍生溶液:5 mg/L三溴化吡啶(TECH)水溶液;衍生液流速:0.3 mL/min;衍生反应器温度:70℃;荧光检测器参数设置为EM=360 nm,EX=440 nm。经检测,黄曲霉毒素总量均有较好的线性关系,线性相关系数r^(2)均大于0.999。检出限在0.01~0.03μg/kg之间。加标回收率为87%~103%。用所建方法同LS/T 6128-2017从时间、样品处理及最后结果上进行对比分析,该方法简单、快速,结果准确,灵敏度高。

Establish a method for the determination of total Aspergillus flavus B and G groups in cereals by two-dimensional liquid chromatography with a simulated post column derivatization system.Uses 68%water,16%acetonitrile,and 16%methanol as mobile phases,with equal elution and a flow rate of 1.0 mL/min;Column temperature:40℃;injection volume:100μL;Derivative solution:5mg/L tribromopyridine(TECH)aqueous solution;Derivative liquid flow rate:0.3mL/min;Derivative reactor temperature:70℃;The fluorescence detector parameter is set to EM=360nm,EX=440 nanometers.The total content of Aspergillus flavus had a good linear relationship,and the linear correlation coefficient r^(2)was greater than 0.999.Detection limit between 0.01~0.03μg/kg.The recovery rate of spiking is 87%-103%.Comparing the established method with LS/T 6128-2017 in terms of time,sample processing,and final results,this method is simple,fast,accurate,and highly sensitive.