固相萃取柱高效液相色谱法检测粮食中玉米赤霉烯酮

建立固相萃取柱净化、高效液相色谱检测粮食中玉米赤霉烯酮方法。样品经乙腈—NaCl溶液(90:10,V/V)超声波提取,固相萃取柱净化,甲醇-水(70:30,V/V)为流动相,流速1 ml/min;荧光检测器检测,激发波长274 nm、发射波长440 nm;柱温30℃;进样量10μl。玉米赤霉烯酮浓度在10～600μg/L范围呈线性,线性回归方程为:Y=5.86 x+23.25,相关系数为0.9997;方法检出限为5μg/kg;3个不同水平加标平均回收率为80.4%～88.5%,相对标准偏差(RSD)为2.5%～5.4%。该法选择性高、净化效果好、操作简单、检测效果理想,适于大批量样品检测,有利于推广。

Determination of zearalenone in grain by solid phase extraction column with high performance liquid chromatography

High performance liquid chromatography(HPLC ) was used for determination of zearalenone in grains.Sample by ultrasonic extraction of acetonitrile:sodium chloride solution (90:10,V/V ),and solid phase extraction column purification.The mobile phase of methanol:water (70:30,V/V),excitation wavelength of fluorescence detector 274 nm and detection wavelength 440 nm. Temperature of column 30℃,and the injection volume of 10μl.The calibration curve is linear in the range of 10—600μg/L,Y=5.86x+23.25,R= 0.9997,The limit of detection was 5μg/kg.The mean recoveries of the spiked at three levels range from 80.4%to 88.5%,and relative standard deviation (RSD ) range from 2.5%to 5.4%.The method has advantages of high selectivity,purification effect, and simplicity of operation,is suitable for determination mass sample,and beneficial promote.