摘要
建立了罐头食品中尿素残留检测的柱前衍生-高效液相色谱-荧光检测方法。取5.0 g样品，经20 mL 1％（ v／v）乙酸溶液提取、定容，离心后取上清液过滤，吸取0.5 mL 提取液用呫吨醇进行衍生，采用高效液相色谱-荧光检测器进行测定。尿素在0.1-500 mg／L内线性良好，相关系数大于0.9995。实验表明，在5种罐头食品中各添加0.001-30 g／kg 尿素，其平均回收率为80.2％-109.7％，相对标准偏差（ n=6）为2.05％-6.53％，检出限为0.5 mg／kg，定量限为1.0 mg／kg。利用本研究建立的方法对168个实际样品进行测定，在3个肉类罐头样品中检出尿素，含量分别为10.6、62.1和2.6 mg／kg。方法稳定、可靠、操作简单，适用于罐头食品中尿素的检测。
A method for the determination of urea residue in canned foods by high performance liquid chromatography-fluorescence detection（ HPLC-FLD）coupled with precolumn derivatiza-tion was established. The sample（5. 0 g）,including canned edible fungi,fruit,vegetable,fish, and meat was extracted with 20 mL 1%（ v/v）acetic acid solution. The extract was centrifuged, filtrated,and then derivatized with xanthydrol. The analysis was completed with HPLC-FLD. A good linear relationship was obtained in the range of 0. 1-500 mg/L with the correlation coeffi-cients more than 0. 999 5. The average recoveries of urea spiked at 0. 001-30 g/kg levels in five kinds of canned foods ranged from 80. 2% to 109. 7% with the RSDs of 2. 05%-6. 53%. The limit of detection（LOD）was 0. 5 mg/kg,and the limit of quantitation（LOQ）was 1. 0 mg/kg. The proposed procedure was then applied to the analysis of 168 real samples collected from Xia-men,Fujian Province,China. The existence of urea was found in three pork cans with contents of 10. 6,62. 1 and 2. 6 mg/kg,respectively. The method is stable,reliable,simple and suitable for the determination of urea in canned foods,and has great potential for routine analysis in foodstuffs.
出处
《色谱》
CAS
CSCD
北大核心
2015年第1期80-83,共4页
Chinese Journal of Chromatography
基金
国家质检总局科技项目(2012IK165)
国家认监委制标项目(2009B739r)
关键词
高效液相色谱
荧光检测
尿素
罐头食品
呫吨醇
high performance liquid chromatography （HPLC）
fluorescence detection （ FLD ）
urea
canned food
xanthydrol
