物料中尿素的测定:使用熟练测试数据评估不同分析技术的适用性
Carlos Gonçalves1, Katrien Bouten1, Pieter Dehouck1
1Joint Research Centre (JRC), European Commission, Geel, Belgium.
概括
在物料中检测尿素的光谱光度法缺乏选择性. 与其他方法不同,液体染色学-并联质谱学 (LC-MS/MS) 证明了在污染物水平上量化尿素的卓越准确性.
科学领域:
- 分析化学 分析化学
- 食品安全 食品安全
- 动物营养 动物营养
背景情况:
- 尿素不是物料中的授权添加剂,但可以非法添加以膨胀明显的蛋白质含量.
- 据报道,目前用于物料中尿素的光谱光度测定方法 (委员会第152/2009/EC条例) 缺乏选择性.
- 精确量化尿素对于经济原因至关重要,并确保遵守料法规.
研究的目的:
- 评估各种分析技术的性能,以确定物料中的尿素在污染物水平.
- 为了比较不同的方法的准确性和可靠性,包括光谱光度测量,LC-MS/MS,HPLC-UV,酶色度测量,重力测量和内部光度测量方法.
- 确定一种适合用于准确确定物料中的尿素的方法,特别是在低度下.
主要方法:
- 组织了一项技能测试,涉及官方控制实验室,学术界和私人实验室.
- 参与者分析了三种狗料试验材料,其中两种材料含不同度的尿素.
- 采用了一系列分析技术,包括光谱光度测量 (执行条例 (EC) 152/2009),LC-MS/MS,HPLC-UV,酶色度测量,重力测量以及"内部光度测量"方法.
主要成果:
- 液体染色学-并联质谱学 (LC-MS/MS) 显示出最高的成功率和准确性,特别是在低水平 (18.9 mg kg−1) 量化尿素时.
- 谱光测量,基于酶的方法和HPLC-UV导致尿素值被高估,结果分散率无法接受.
- 通过LC-MS/MS,一种"内部光度法",以及在较高尿素度 (258.9毫克/公斤-1) 的酶法获得了令人满意的结果.
结论:
- 现行法规规定的光谱光度法不适合在物料中的尿素在污染物水平的选择性确定.
- LC-MS/MS是准确量化物料中的尿素的最可靠技术,特别是在低度下.
- 对于物料中尿素的合规性监测,需要比目前的立法方法更有效的分析方法.
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