免疫亲和柱净化—液相色谱法测定玉米油中的玉米赤霉烯酮含量
目的 建立免疫亲和柱净化—液相色谱法测定玉米油中玉米赤霉烯酮含量的分析方法。方法 样品采用乙腈-水(9:1, V:V)提取, 免疫亲和柱净化, 经Inertsil ODS3-C18柱 (250 mm×4.6 mm, 5 μm)分离, 以乙腈-水-甲醇(46:46:8, V:V:V)为流动相进行等度洗脱, 流速1.5 mL/min, 柱温30 ℃, 经荧光检测器检测, 外标法定量。结果 玉米赤霉烯酮在25~2500 μg/kg范围内具有良好线性, 相关系数为0.99998, 检出限5 μg/kg, 加标回收率为87.5%~107.5%, 相对标准偏差为3.2%~5.8%。对调和油中米赤霉烯酮质控考核样品Mycotoxin-PT-2018-042的检测结果满意。结论 该方法前处理操作简便, 损失少, 减少了试剂用量, 灵敏度高, 准确度高, 适用于玉米油中玉米赤霉烯酮的检测。
Objective To establish a method for the determination of zearalenone in corn oil by immunoaffinity column purification-liquid chromatography. Method The sample was extracted with acetonitrile-water (9:1, V:V) and purified by immunoaffinity column, separated with Inertsil ODS3-C18 column (250 mm×4.6 mm, 5 μm) at the flow rate of 1.5 mL/min by isocratic elution using acetonitrile-water-methanol (46:46:8, V:V:V) as mobile phase. The temperature of the column oven was maintained 30 ℃ and the signal was detected with fluorescence detector. The zearalenone content was quantitatively analyzed by external standard method. Results The zearalenone had good linear relationships in the range of 25~2500 μg/kg, and the correlation coefficient was 0.99998. The limit of detection was 5 μg/kg. The standard recovery rate was 87.5%?107.5%, with the relative standard deviations of 3.2%?5.8%. The results of the test of Mycotoxin-PT-2018-042 in the quality control sample of gibberellin in the blended oil were satisfactory. Conclusion This method has the advantages of simple pretreatment, less loss, reduced reagent dosage, high sensitivity and high accuracy, and is suitable for the detection of zearalenone in corn oil.
标题：免疫亲和柱净化—液相色谱法测定玉米油中的玉米赤霉烯酮含量
英文标题：Determination of zearalenone in corn oil by immunoaffinity column purification and liquid chromatography
作者：
张昆仑 大理州疾病预防控制中心
陈晓明 大理州疾病预防控制中心
刘玉娇 大理州疾病预防控制中心
虞震 大理州疾病预防控制中心
李云升 大理州疾病预防控制中心
中文关键词:玉米赤霉烯酮,液相色谱法,免疫亲和柱净化,玉米油,
英文关键词:zearalenone,liquid chromatography,immunoaffinity column clean up,corn oil,
发表日期：2019-08-22
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