奶中氯霉素残留量的高效液相色谱方法研究

Determination of Chloramphenicol Residues in Milk by High Performance Liquid Chromatography Method

建立了对牛奶中氯霉素残留量进行检测的高效液相色谱-荧光测定方法的研究。氯霉素还原后在温和条件下与荧光胺发生衍生化反应，采用十八烷基键合硅胶固定相，以乙腈／四氢呋喃／（0．02mol／L）醋酸钠-醋酸缓冲液（pH=6．0）为流动相，用荧光检测。氯霉素检测的线性范围为0．2～8009g／L（r=0．9997），检出限为0．1μg几。回收率96．3％～102．7％，相对标准偏差1．2％～3．6％。该方法适用于牛奶中氯霉素痕量残留的检测，具有干扰小、选择性好、灵敏度高等优点。

A high performance liquid chromatographic method with fluorescence detection for the determination of chloramphenicol（CAP） residues in milk was developed. The aromatic nitro group of CAP could be reduced to aromatic primary amino group, and fluorescamine can be used as a selective reagent for primary amines. Therefore, the CAP was derivatized with fluorescamine prior to injection in this project. The HPLC method was performed on a Diamond C18 column with the mobile phase composed of sodium acetate buffer （0.02mol/ L, pH = 6.0） acetonitrile tetrahydrofuran. Analytes were detected by a fluorescence detector. The standard curve was linear in the range from 0.2μg/L to 800 μg/L （r = 0.9997）. The limit of detection was 0. 1μg/L. Over all recoveries were between 96.3% - 102.7% with relative standard deviations between 1.2% - 3.6%. The procedure provides a rapid, reliable and sensitive method for the determination of CAP in milk.