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Determination of ergot alkaloids in feed by HPLC

机译:高效液相色谱法测定饲料中麦角生物碱

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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).
机译:建立了一种高效液相色谱法测定动物饲料和高谷物混合饲料谷物中的麦角新碱,麦角胺,麦角新碱,α-麦角隐碱和麦角碱。在酸性条件下,使用磷酸和乙腈的混合物萃取样品,萃取物用固相萃取柱纯化(强阳离子交换),并通过HPLC在C18色谱柱上梯度洗脱,通过荧光检测法检测麦角生物碱。每种生物碱的检出限和测定限分别为5(μ/ kg和10(μg/ kg)。通过这种方法,小麦,黑麦和混合饲料的高回收率(82–120%)和良好的重现性达到了总测定的生物碱总量<500(μg/ kg。该方法用于分析三年(2005-2007年)的巴伐利亚饲料(n = 124),并且在91%的样品中检出了麦角生物碱。的阳性样品中麦角生物碱含量<250μg/ kg,中性生物碱水平为70(μg/ kg。在小麦,黑小麦,黑麦和混合饲料中,总测定生物碱的总和超过1000(μg/ kg,混合饲料(4880(μg/ kg))获得最高结果。

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