反刍动物配合饲料中尿素的测定:委员会法规(EC) No 152/2009分光光度法验证的实验室间比较

C. Gonçalves, K. Bouten, H. Emteborg, J. Stroka, C. Holst, U. Vincent
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引用次数: 3

摘要

主题描述。尿素是经批准用于反刍动物饲料的饲料添加剂,配合饲料中尿素的最大含量为8800 mg·kg-1。欧盟委员会法规(EC) No 152/2009显示了测定饲料中尿素的官方方法,但没有指定该方法适用的饲料类型。成员国的报告指出,官方分光光度法不适用于反刍动物饲料以外的饲料,并且考虑到没有确定方法的性能特征,联合研究中心组织了一次实验室间的演习来验证该方法。目标。目的是根据欧盟委员会DG SANTE的具体要求,开展一项实验室间环试验,以验证用于测定反刍动物配合饲料中尿素的官方分光光度法。方法。以含尿素不同质量分数的反刍动物配合饲料为原料,制备了6种不同的试验材料和一种空白试验材料。19个实验室参加了这项研究,来自10个欧盟成员国的18个实验室提交了结果。结果。建立了性能特征,即本研究使用的验证标准(RSDR)在所有情况下均达到(即低于20%),除了在420 nm测量的3,000 mg·kg-1绵羊饲料中。在435 nm处获得了稍好的精密度和准确度。结论。欧盟委员会法规(EC) No 152/2009应对官方分光光度法进行修订,并限制其范围,即在授权水平下测定反刍动物复合饲料中的尿素。此外,所选择的测量波长(420 nm或435 nm)对该方法的性能影响较小。
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Determination of urea in compound feed for ruminants: interlaboratory comparison for the validation of the spectrophotometric method in Commission Regulation (EC) No 152/2009
Description of the subject. Urea is a feed additive authorized in ruminant feedingstuff with a maximum content in compound feed of 8,800 mg·kg-1. Commission Regulation (EC) No 152/2009 displays the official method for the determination of urea in feed but does not specify the type of feed for which the method is applicable. Following reports from Member States stating that the official spectrophotometric method is not fit for purpose for other feed than ruminant feed and given the fact that no method performance characteristics are set, the Joint Research Centre organized an interlaboratory exercise for the validation of this method. Objectives. The objective was to carry out an interlaboratory ring trial for the validation of the official spectrophotometric method for the determination of urea in compound feed for ruminants, under specific request from DG SANTE of the European Commission. Method. A collaborative study was carried out on six different test materials prepared from ruminant compound feeds containing urea at various mass fractions and a blank test material. Nineteen laboratories enrolled for the study and eighteen laboratories from ten EU Member States submitted results. Results. The performance characteristics were established, namely, the validation criterion used in this study (RSDR) was in all cases, except in sheep feed at 3,000 mg·kg-1 measured at 420 nm, achieved (i.e. lower than 20%). Slightly better results in terms of precision and trueness were obtained at 435 nm. Conclusions. Commission Regulation (EC) No 152/2009 should be revised as regards the official spectrophotometric method with a restriction of the scope, which is the determination of urea in ruminant compound feedingstuff at authorized level. Additionally, the selected measurement wavelength, which is either 420 nm or 435 nm, has a minor impact on the performance profile of the method.
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