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以乙腈和NaCl溶液为提取剂提取玉米赤霉烯酮,固相萃取柱净化,高效液相色谱法荧光检测器检测。通过单因素和正交实验,探讨了料液比、乙腈∶NaCl溶液比、NaCl浓度、超声提取时间对提取效果的影响,得到最佳提取条件为料液比25∶100、乙腈∶NaCl溶液比80∶20、NaCl溶液浓度为40g/L、超声提取时间为15min;通过对固相萃取柱净化条件、液相色谱流动相、流速、柱温选择优化,得到以甲醇-水为流动相,甲醇与水比例为65∶35(v/v)、流速为1mL/min、柱温为30℃时,检测效果最好;通过对检测方法日内、日间加标回收实验,得到该检测方法回收率为78.2%～89.6%,相对标准偏差为1.5%～3.9%;检测限为8μg/kg。该方法简便快速,重现性好,适合于玉米赤霉烯酮的实际检测应用。
The zearalenone was extracted with acetonitrile and NaCl as the extractant, purified by solid phase extraction (SPE) and detected by high performance liquid chromatography with fluorescence detector. Through the single factor and orthogonal experiment, the effects of the ratio of solid to liquid, the ratio of acetonitrile to NaCl solution, the concentration of NaCl and the time of ultrasonic extraction on the extraction were discussed. The optimal extraction conditions were as follows: the ratio of solid to liquid was 25:100, the ratio of acetonitrile to NaCl solution 80:20, the concentration of NaCl solution 40g / L, ultrasonic extraction time 15min; by solid phase extraction column purification conditions, liquid chromatography mobile phase, flow rate, column temperature optimization, methanol to water as the mobile phase, methanol Water ratio of 65:35 (v / v), the flow rate of 1mL / min, the column temperature of 30 ℃, the detection effect is best; by the detection method of days and days plus standard recovery test, the detection method recovery Was 78.2% ~ 89.6% with relative standard deviation of 1.5% ~ 3.9%. The detection limit was 8μg / kg. The method is simple and rapid, reproducible, suitable for the actual detection of zearalenone.