Bavarian Health and Food Safety Authority, Veterinärstr. 2, 85764, Oberschleißheim, Germany,
Mycotoxin Res. 2008 Jun;24(2):73-9. doi: 10.1007/BF02985284.
A HPLC method for the determination of ergometrine, ergotamine, ergocristine, α-ergocryptine and ergocornine in cereals for animal feed and in mixed feed with high cereal content was developed. Samples were extracted under acidic conditions using a mixture of phosphoric acid and acetonitrile, the extract purified with solid phase extraction cartridges (strong cation exchange), and ergot alkaloids detected after gradient elution on a C18 column by HPLC with fluorescence detection. Detection and determination limits for each individual alkaloid were at 5 (μ/kg and 10 (μg/kg, respectively. With this method, high recovery (82-120%) and good reproducibility was achieved for wheat, rye and mixed feeds, at a sum of total determined alkaloids of < 500 (μg/kg. This method was used to analyse Bavarian feeds (n=124) over three years (2005-2007), and ergot alkaloids were detected in 91 % of the samples. The majority of positive samples had ergot alkaloid contents of < 250 μg/kg, the median alkaloid level was at 70 (μg/kg. The maximum sum of total determined alkaloids exceeded 1000 (μg/kg in wheat, triticale, rye, and mixed feeds, the highest result was obtained for mixed feed (4880 (μg/kg).
开发了一种用于测定动物饲料用谷物和高谷物含量混合饲料中麦角新碱、麦角胺、麦角克碱、α-麦角隐亭和麦角柯宁的 HPLC 方法。样品在酸性条件下用磷酸和乙腈的混合物提取，用固相萃取小柱（强阳离子交换）纯化提取物，然后通过 HPLC 荧光检测在 C18 柱上进行梯度洗脱后检测麦角生物碱。每种生物碱的检测和测定限分别为 5（μ/kg 和 10（μg/kg。使用该方法，小麦、黑麦和混合饲料的回收率（82-120%）高且重现性好，总测定的生物碱含量<500（μg/kg。该方法用于分析巴伐利亚饲料（n=124）三年（2005-2007 年），91%的样品中检测到麦角生物碱。大多数阳性样品的麦角生物碱含量<250μg/kg，生物碱水平中位数为 70（μg/kg。在小麦、小黑麦、黑麦和混合饲料中，总测定的生物碱总量的最大值超过 1000（μg/kg，最高结果为混合饲料（4880（μg/kg）。
