摘要
本文建立了谷物及其制品中玉米赤霉烯酮免疫亲和-高效液相色谱分析方法。样品经乙腈-去离子水(体积比84∶16)提取,玉米赤霉烯酮免疫亲和柱富集净化,甲醇洗脱,高效液相色谱-荧光检测器检测,C18反相色谱柱分离,流动相为乙腈-水-甲醇(体积比46∶46∶8),保留时间定性,外标法定量。结果显示,该方法的线性范围为1~100μg/L,相关系数为0.9999,检出限为0.8μg/kg,2个不同水平的添加回收率为91.3%~99.5%,仪器重复测定的相对标准偏差为0.19%,样品平行性测定相对标准偏差为0.10%~1.89%。由此得出,该方法具有线性范围宽、灵敏度高、重现性好、准确度高、适应性强等特点,符合谷物及其制品中痕量分析的要求。
This paper builds a method of immunoaffinty and high efficiency liquid chromatography which tested the concentration of the zearalenone in the grain and its products in market.The samples are extracted by the mixture of acetonitrile and deionized water(volume ratio is 84:16).The extract is cleaned-up and concentrated by the zearalenone immuno affinity column,eluted by methyl alcohol,and detected by the high performance liquid chromatography with fluorescence detector.People also adopted the C18 reversed phase column to separate the compound,and the mobile phase are acetonitrile-water-methyl alcohol(volume ratio is 46:46:8).The retention time of the peaks is used for qualitative analysis,while external standard method is used for quantitative analysis.The results show that the method linearity range is 1—100μg/L,the correlation coefficient is 0.9999,the limit of detection is 0.8μg/kg,the add recoveries of the two levels are 91.3%—99.5%,the relative standard deviation of the instrument detection is 0.19%,while the relative standard deviation of the samples parallel determination is 0.10%—1.89%.It is concluded that the method has the characteristics of wide linear range,high sensitivity,good reproducibility,high accuracy and strong adaptability,and it is in line with the requirements of trace analysis in grain and its products.
作者
耿振
姜延国
尹晶
GENG Zhen;JIANG Yanguo;YIN Jing(Dandong Health Service Center,Dandong,Liaoning,118000,China)
出处
《检验检疫学刊》
2019年第5期61-62,共2页
Journal of Inspection and Quarantine
