Muñiz-Valencia R, Ceballos-Magaña S G, Gonzalo-Lumbreras R, Santos-Montes A, Izquierdo-Hornillos R
Departamento de Química Analítica, Facultad de Ciencias Químicas, Universidad Complutense, 28040, Madrid, Spain.
Anal Bioanal Chem. 2008 Aug;391(7):2683-91. doi: 10.1007/s00216-008-2176-8. Epub 2008 May 28.
An HPLC-DAD method for determining corticoids in calf feed and in animal feeding water samples using a monolithic column has been developed and validated. The method optimization included the study of binary mobile phases of water and acetonitrile. The optimum separation was achieved at 40 degrees C, with acetonitrile:H(2)O 29:71 v/v used as mobile phase and a 3 ml/min flow-rate, which resulted in their separation in about 5 min. Two reported sample procedures were applied to feed and for animal feeding water samples prior to HPLC. Method validation was carried out according to the EU criteria established for quantitative screening methods. The results indicate that this method is highly specific, reproducible and accurate. The proposed method was found to be robust and unaffected by small variations in the extraction procedure and in HPLC conditions. The developed method for the determination of corticoids in feed and water samples was also found to be suitable for different kinds of feeds and waters.
已开发并验证了一种使用整体柱测定小牛饲料和动物饮用水样品中皮质激素的HPLC-DAD方法。方法优化包括对水和乙腈二元流动相的研究。在40℃下实现了最佳分离，以乙腈:水29:71 v/v作为流动相，流速为3 ml/min，约5分钟内实现了它们的分离。在进行HPLC分析之前，将两种已报道的样品处理程序应用于饲料和动物饮用水样品。根据为定量筛选方法制定的欧盟标准进行方法验证。结果表明该方法具有高度特异性、可重复性和准确性。所提出的方法被发现具有稳健性，不受提取程序和HPLC条件的微小变化影响。所开发的用于测定饲料和水样中皮质激素的方法也被发现适用于不同种类的饲料和水。
