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作 者:陈冉 邱艳 都晓慧 管平 许建华 吴秋蓉 朱贞映 涂文博 郭亚鹏 郭腾龙 Chen Ran;Qiu Yan;Du Xiaohui;Guan Ping;Xu Jianhua;Wu Qiurong;Zhu Zhenying;Tu Wenbo;Guo Yapeng;Guo Tenglong(Sinograin Hubei Branch Quality Inspection Center Co.,Ltd 430311;Linshu County Market Supervision and Management Comprehensive Law Enforcement Brigade,276799)
机构地区:[1]中储粮湖北质检中心有限公司,430311 [2]临沭县市场监督管理综合执法大队,276799
出 处:《粮食储藏》2023年第3期39-42,共4页Grain Storage
摘 要:通过优化液相色谱检测条件,简化前处理操作步骤,探索一种简单、快速、高效、无需氮吹检测粮食中呕吐毒素的方法。样品经水提取,振荡、过滤后,过免疫亲和柱净化,用甲醇洗脱,加水混匀,采用高效液相色谱仪检测。调整进样溶液中甲醇与水的比例,比较色谱峰峰形,研究发现,当进样溶液中甲醇与水的比例为1∶0.8时,呕吐毒素色谱峰形最佳,对称因子接近于1.0。通过调整流动相中有机相比例,评价呕吐毒素在色谱柱中的保留行为,结果表明,随着流动相中有机相比例的增加,保留时间缩短,当甲醇水体系中甲醇比例为18%,或乙腈水体系中乙腈比例为8%时,呕吐毒素出峰时间适中,在5 min~10 min内,与死时间和杂质峰完全分离,峰形对称性好。The study explored,a simple,that was a rapid and efficient method by optimizing the detection to check the deoxyniverenol in grain without nitrogen blowing by optimizing the detection conditions of liquid chromatography and simplifying the operation steps of pretreatment.The samples were extracted with water,oscillated,filtered,purified by immunoaffinity columns,eluted with methanol,mixed with water,and detected by HPLC.Adjusted the ratio of methanol&water in the sample solution,then compared the chromatographic peaks shape,we found that when the ratio of methanol&water was 1∶0.8,the chromatographic peak shape of deoxyniverenol was the best,and the symmetry factor was close to 1.0.We evaluated the retention behavior of deoxyniverenol crosing the chromatographic column by adjusting the proportion of organic phase in the mobile phase,the results showed that with increasing the proportion of organic phase in the mobile phase,the retention time was shortened.When the proportion of methanol in methanol water system was 18%,or the proportion of acetonitrile in acetonitrile water system was 8%,the retention time of deoxyniverenol was moderate within 5-10 minutes,the peak was completely separated from dead time and impurity peak with good symmetric.
分 类 号:TS210.7[轻工技术与工程—粮食、油脂及植物蛋白工程]
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