高效液相色谱测定乳制品、谷物粉及饲料中脱氧雪腐镰刀菌烯醇及其乙酰化衍生物

High Performance Liquid Chromatography Determination of Deoxynivalenol and Its Acetyl Derivatives in Dairy Products, Cereal Flour and Dairy Cow Feed

建立乳制品、谷物粉和饲料中脱氧雪腐镰刀菌烯醇(deoxynivalenol,DON)及其衍生物3-乙酰基-脱氧雪腐镰刀菌烯醇(3-acetyl-deoxynivalenol,3-ADON)和15-乙酰基-脱氧雪腐镰刀菌烯醇(15-acetyl-deoxynivalenol,15-ADON)的高效液相色谱检测方法。样品经超纯水提取、免疫亲和柱净化,紫外检测器检测。结果表明:乳制品、谷物粉和饲料中DON、3-ADON和15-ADON的定量限均为100?μg/kg;DON的添加量在100～500?μg/kg范围内时,其在乳制品、谷物粉和饲料中的回收率均大于90%;3-ADON和15-ADON的添加量在100～500?μg/kg范围内时,其在乳制品、谷物粉和饲料中的回收率均在80%以上,方法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,可以同时检测饲料、乳制品和谷物粉中DON、3-ADON和15-ADON的含量。

A method for the determination of deoxynivalenol (DON) and its derivatives 3-acetyl-deoxynivalenol (3-ADON) and 15-acetyl-deoxynivalenol (15-ADON) in dairy products, cereal flour and dairy cow feed was developed using high performance liquid chromatography (HPLC). Samples were extracted with ultrapure water, and the extract was cleaned up by immunoaffinity column chromatography and detected by HPLC with ultraviolet detection (HPLC-UVD). The limit of quantitation of the method was 100 μg/kg for all three analytes in dairy products, cereal flour and feed. Recoveries from these three sample matrices spiked at concentration levels ranging from 100 to 500 μg/kg were higher than 90% for DON and higher than 80% for 3-ADON and 15-ADON. This method proved to be simple, fast, sensitive, highly selective, and suitable for the simultaneous analysis of DON, 3-ADON and 15-ADON in dairy products, cereal flour and feed.