引用本文:王培,徐广超,尹丽梅,黎睿,谢刚.免疫亲和柱净化—高效液相色谱法同时检测小麦中脱氧雪腐镰刀菌烯醇及其衍生物[J].粮油食品科技,2015,23(1):63-66.
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免疫亲和柱净化—高效液相色谱法同时检测小麦中脱氧雪腐镰刀菌烯醇及其衍生物
王培1, 徐广超2, 尹丽梅3, 黎睿4, 谢刚4
1.山东省粮油检测中心,山东 济南253303;2.国家粮食局标准质量中心,北京100037;3.北京华安麦科生物技术有限公司,北京102002;4.国家粮食局科学研究院,北京100037
摘要:
建立脱氧雪腐镰刀菌烯醇(DON)及其衍生物3-乙酰基—脱氧雪腐镰刀菌烯醇(3-A-DON)和15-乙酰基—脱氧雪腐镰刀菌烯醇(15-A-DON)的免疫亲和柱净化—高效液相色谱同时检测方法。小麦样品经超纯水提取、免疫亲和柱净化、吹干、定容后,用配有紫外检测器的高效液相色谱仪进行DON、3-A-DON和15-A-DON三种毒素的同时检测,并与液相色谱质谱法比对。结果表明:该方法检出限,DON、3-A-DON和15-A-DON均为100 μg/kg,样品加标回收率范围86.6% ~ 96.5%,变异系数小于10%,具有较好的准确性和精密度。该方法简单、快速、灵敏度高、选择性好,适用于小麦中DON、3-A-DON和15-A-DON的同时检测。
关键词:  免疫亲和柱  脱氧雪腐镰刀菌烯醇  3-乙酰基—脱氧雪腐镰刀菌烯醇  15-乙酰基—脱氧雪腐镰刀菌烯醇  高效液相色谱
DOI:
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基金项目:
Simultaneous determination of deoxynivalenol and ramification in wheat by immune affinity column and high performance liquid chromatography
Abstract:
The method to determine deoxynivalenol (DON), 3-acetyl- deoxynivalenol (3-A-DON) and 15-acetyl-deoxynivalenol (15-A-DON) in wheat simultaneously by immune affinity column clean-up and high performance liquid chromatography was established. The wheat samples were extracted by ultrapure water, cleared up with the immuno-affinity column (IAC). After drying and constant volume, three toxins, DON、3-A-DON and15-A-DON, were detected simultaneously by high performance liquid chromatograph with UV detector, and compared with that by Liquid chromatography mass spectrometry. The result showed that the detection limit of method was 100 μg/kg for DON, 3-A-DON and 15-A-DON respectively. Recovery rates in wheat spiked with DON, 3-A-DON, and 15-A-DON, ranged from 86.6% to 96.5%. The variation coefficient was less than 10%. This method was suitable for determination of DON, 3-A-DON, and 15-A-DON in wheat, with the advantages of simplicity, rapidness, sensitivity and good selectivity, veracity and precision.
Key words:  immune affinity column  deoxynivalenol(DON)  3-acetyl-deoxynivalenol  15-acetyl-deoxynivalenol  high performance liquid chromatography