摘要
为建立高效液相色谱-串联质谱同时测定运动马饲粮中15种真菌毒素含量的分析方法 ,样品经乙腈-甲酸(V/V,9∶1)溶液进行超声提取15 min,提取液经B组净化剂(150 mg C18+150 mg PSA+200 mg GCB)净化处理后上机分析。分析液采用C18色谱柱进行分离,以15 mmol/L乙酸铵水溶液和乙腈作为流动相进行梯度洗脱。结果表明:在相应浓度范围内15种真菌毒素具有良好的线性关系,其相关系数(r)≥0.9967,方法检出限为0.041~2.178μg/kg;定量限为0.151~8.945μg/kg。分别向阴性样品中添加低、中、高3水平加标浓度,15种真菌毒素的加标平均回收率为76.65%~98.56%;其相对标准偏差(RSDs)为0.154%~9.894%(n=6)。该方法简单、快速、灵敏,可以作为饲料中多类真菌毒素的快速筛查和确证方法。
The aim of this experiment was to establish an method for simultaneously determinating of 15 mycotoxins in sports horse food by HPLC-MS/MS.The samples were ultrasonic extracted by acetonitrile formic acid(V/V,9∶1)solution for 15 min.The extracted solution was purified by group B purification agent(150 mg C18+150 mg PSA+200 mg GCB)and then analyzed on the machine.The analytical solution was separated by C18 column and gradient elution was performed with 15 mmol/L ammonium acetate aqueous solution and acetonitrile as mobile phase.The results showed that the correlation coefficient(r)was≥0.9967.The detection limit was 0.041~2.178μg/kg,and the limits of quantification was 0.151~8.945μg/kg.The average recoveries of 15 mycotoxins were 76.65%~98.56%when low,medium and high 3 levels were added to negative samples respectively.The relative standard deviation(RSDs)ranged from 0.154%to 9.894%(n=6).The method was simple,rapid and sensitive,and could be used as a rapid screening and confirmation method for many kinds of mycotoxins in feed.
作者
曹海园
鲍娟
唐云豪
孙金梁
CAO Haiyuan;BAO juan;TANG Yunhao;SUN Jinliang(Zaozhuang University,Zaozhuang,Shandong Province 277100,China;Yancheng Preschool Teachers College,Yancheng,Jiangsu Province 224069,China;Department of Public Physical Education and Research,Changchun University of Humanities,Changchun,Jilin Province 130000,China)
出处
《中国饲料》
北大核心
2025年第17期122-129,共8页
China Feed
基金
山东省重大科技创新工程项目(2019JZZY020602)。
