高效液相色谱法测定玉米赤霉烯酮的方法研究  

Determination method of zearalenone by means of high-performance liquid chromatography

作　　者：罗小虎[1] 包清彬[1] 杨潇[1] 孔凌[1] 

机构地区：[1]西华大学生物工程学院,成都610039

出　　处：《食品科技》2010年第1期266-270,共5页Food Science and Technology

基　　金：国家粮食局"十一五"科技支撑计划项目(2006BAD08B07);四川省重点学科建设项目

摘　　要：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。Acetonitrile and NaCI solution for the extraction solvent extracted zearalenone, solid-phase extraction column purification, high performance liquid chromatography fluorescence detection. By single factor and orthogonal experiment, we studied the proportion of solid-liquid, acetonitrile and NaCI solution ratio, NaCI concentration and ultrasonic extraction time on extraction effect. The best conditions of the solid-liquid ratio is 25：100, acetonitrile and NaCI solution ratio is 80：20, NaCI concentration is 40 g/L and ultrasonic extraction time 15 min.By optimization of choice solid-phase extraction purification conditions, mobile phase, flow rate, column temperature, The results of methanol-water as the mobile phase and proportion is 65：35（v/v）, flow rate is 1 mL/ min, column temperature 30℃, detection effect the best; recovery experiment by within-day and inter-day added standard, recoveries of 78.2-89.6%, relative standard deviation of 1.5%-3.9%, the detection limit was 8 μg/kg. The method is simple and fast, good reproducibility, suitable for zearalenone detection the actual application.

关 键 词：玉米赤霉烯酮 玉米 高效液相色谱 固相萃取 

分 类 号：O657.7[理学—分析化学]