高效液相色谱法测定饲料及食品中三聚氰胺的研究(1)
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[摘要] 目的:建立用高效液相色谱-二极管阵列法(HPLC-DAD)测定饲料及食品中三聚氰胺残留量的方法。方法:样品经提取分离后,用HPLC-DAD法测定,外标法定量。色谱条件:C18色谱柱(150 mm×4.6 mm,5 μm);流动相为乙腈-辛烷磺酸钠溶液(柠檬酸调节pH至3.0,10∶90),流速为1.0 ml/min;进样量为20 μl;柱温为35℃;190~400 nm波段扫描,检测波长为236 nm。结果:三聚氰胺在0.5～10.0 μg/ml范围内线性关系良好,相关系数R=0.999 98。最低检测浓度为0.05 μg/ml,回收率在89.28%～96.89%范围内,RSD<3.5%。结论:该方法简便、快速,能满足饲料及食品中三聚氰胺残留量的检验工作需要。
[关键词] 三聚氰胺;奶制品;饲料;鸡蛋;高效液相色谱法
[中图分类号] O642.5[文献标识码]A [文章编号]1673-7210(2010)06(c)-012-03
Determination of melamine residue in feed and food by HPLC
LIU Hongju1, YAN Chong1, LI Guoliang1, ZHOU Peiling1, LIU Hongguo2
(1.School of Pharmacy, Guangdong Medical College, Dongguan 523808, China; 2.Hebei Ideal & Hightech Pharmaceutical Corporation Limited, Shijiazhuang 050021, China)
[Abstract] Objective: To establish a method for the determination of melamine residue in feed and food using high performance liquid chromatography-diode array detection (HPLC-DAD). Methods: After the sample was extracted and cleaned, melamine was analyzed by HPLC-DAD. Using C18 column (150 mm×4.6 mm, 5 μm), acetonitrile and 10 mmol/L sodium octanoate solution (adjusted pH to 3.0 with acetic acid, 10∶90) were used for this method. The flow rate was 1.0 ml/min and DAD detection at 236 nm. The temperature of the column was 35℃. Results: The linear range was 0.5-10.0 μg/ml, and the correlation coefficient was 0.999 98. The limit of melamine ranged from 89.28%-96.89% with relative standard deviation (RSD) less than 3.5%. Conclusion: The results indicate that this method is simple and quick, and can meet the requirement for determination of melamine in feed and food.
[Key words] Melamine; Diary products; Feed; Egg; HPLC
三聚氰胺是一种重要的含氮杂环有机化工原料,为尿素后加工产物,主要用途是作为生产三聚氰胺甲醛树脂(NF)的原料,而且还能用作阻燃剂、减水剂、甲醛清洁剂。三聚氰胺的含氮量为66.6%,折合粗蛋白含量为416.27%,添加到饲料及食品中可大幅度提高蛋白含量指标,但也能引发肾衰竭并导致死亡。2007年3月,美国发生了宠物饲料导致猫狗致死的事件,而后在回收的宠物食品、死亡动物的尿液结晶和肾脏中都发现有三聚氰胺。2008年9月,我国发生了“三鹿奶粉事件”,此次事件的原因是奶农为提高牛奶中的蛋白含量指标,在其中添加了三聚氰胺,致使大量婴儿摄入过量的三聚氰胺,全国范围内大量婴儿出现肾脏功能障碍,部分婴儿甚至出现肾衰竭而死亡。在对其他奶制品和鸡蛋等食品进行抽样检查时也检测出了三聚氰胺。为了保证人们的身体健康,确保食品安全,企业和食品安全监管部门必须对食品和饲料中的三聚氰胺进行检测 ......
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