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.
参考文献
| [1] | Deng H P,Zhang H Y,Lü Y Q,et al. Chinese Journal of Health Laboratory Technology(邓辉萍,张红宇,吕玉琼,等. 中国卫生检验杂志),2001,11(5):591,2001. |
| [2] | Qi G Y,Zhao G Y,Song Y H,et al. Chinese Journal of Health Laboratory Technology(齐国艳,赵桂艳,宋彦辉,等. 中国卫生检验杂志),2008,18(11):2397,2008. |
| [3] | Wei F,Ma Z S,Jia Z H. Food Engineering(魏峰,马振山,贾中辉. 食品工程),2006(1):58,2006. |
| [4] | Wang X J,Fu L,Li J F,et al. Science and Technology of Food Industry(王晓娟,傅力,李建飞,等. 食品工业科技), 2009,30(5):317,2009. |
| [5] | Wang Y B,Li Y Z,Hao W Q,et al. China Dairy Industry(王余波,李延昭,郝卫强,等. 中国乳品工业),2011,39(7):50,2011. |
| [6] | Clark S,Francis P S,Conlan X A,et al. J Chromatogr A, 2007,1161:207,2007. |
| [7] | Xing J T,Zhong Q D,Xiong Z H,et al. Liquor-making Sci-ence &Technology(邢江涛,钟其顶,熊正河,等. 酿酒科技),2011(3):104,2011. |
| [8] | Zhang J,Liu G X,Zhang Y,et al. J Agric Food Chem, 2014,62:2797,2014. |
| [9] | Wang Z X,Jiang J,Sun L,et al. Journal of Instrumental Analysis(王祖翔,蒋俊,孙莉,等. 分析测试学报),2012, 31(5):593,2012. |
| [10] | Dai X H,Fang X,Su F H,et al. J Chromatogr B,2010, 878:1634,2010. |
| [11] | Yang R J,Liu R,Xu K X. Spectroscopy and Spectral Analy-sis(杨仁杰,刘蓉,徐可欣. 光谱学与光谱分析),2011,31 (9):2383,2011. |
| [12] | Trivedi U B,Lakshminarayana D,Kothari I L,et al. Sen-sors Actuat B-Chem,2009,140:260,2009. |
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