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饲料中玉米赤霉烯酮的提纯与测定
Purification and detection of zearalenone in feedstuff
【摘要】 玉米赤霉烯酮污染饲料对人、畜造成巨大威胁,因此,对饲料中玉米赤霉烯酮检测水平的提高已不容忽视。为玉米赤霉烯酮监控提供灵敏、可靠的分析方法和试验数据,对其提纯与高效液相色谱测定方法进行了研究,结果表明:样品纯化条件,以二氯甲烷和NaCl溶液为提取剂,湿填硅胶柱为富集净化柱,用6 ml的甲醇溶液洗脱,采用HPLC进行测定;高效液相色谱检测条件,流动相为甲醇/水(80∶20,体积比),流速为0.6 ml/min,紫外检测波长为236 nm,此时最低检出限为5μg/kg,在1.25~40.00μg/ml范围内,被测物浓度与测定的峰面积呈线性关系(r=0.999 1);通过对检测方法日内、日间加标回收试验得到该检测方法回收率约为96.3%。该方法简便、快速、准确,可适用于饲料中玉米赤霉烯酮的提纯与测定。
【Abstract】 Zearalenone contamination of feedstuff causes a great damage to people and livestock.Raising its purification and detection levels should not be ignored.To provide a sensitive and reliable analytical method,purification and determination of zearalenone contaminant in feedstuff by HPLC(high performance liquid chromatography) were optimized.The sample was extracted by methanol and NaCl solution and further purified by a wet fill with silica gel column,which was eluted by 6 ml methanol solution.The target compound was assayed by HPLC,whose optimized condition was as follows: the mobile phase was methanol/water(80/20,V/V),flow rate was 0.6 ml/min,and detection wave was 236 nm.So the detection limit was 5 μg/kg.The relationship of zearalenone concentration and peak area was linear in the range of 1.25~40.0 μg/ml(r=0.999 1).The recovery rate was 96.3% tested by within-day and inter-day added standard experiments.It indicated that the established method was simple,rapid and accurate,which could be used for the determination of zearalenone in foodstuff.
【Key words】 zearalenone; purification; detection; high performance liquid chromatography;
- 【文献出处】 江苏农业学报 ,Jiangsu Journal of Agricultural Sciences , 编辑部邮箱 ,2011年03期
- 【分类号】S816.17
- 【被引频次】7
- 【下载频次】420