鸡蛋和牛奶中噁喹酸、氟甲喹残留的检测方法研究

Detection Method of Oxolinic Acid and Flumequine Residues in Eggs and Milk

关键词:  噁喹酸  氟甲喹  残留  鸡蛋  牛奶  高效液相色谱

Key words:  oxolinic acid  flumequine  residues  eggs  milk  HPLC

摘要:

建立了高效液相色谱-荧光检测器法测定鸡蛋和牛奶中噁喹酸和氟甲喹残留量的方法。用1%甲酸乙腈提取样品中噁喹酸和氟甲喹残留；HPLC条件：C18色谱柱，流动相为0.02 mol/L磷酸溶液-乙腈-四氢呋喃（68∶16∶16）；检测波长：激发波长325 nm，发射波长369 nm。结果显示，噁喹酸和氟甲喹在3~500 ng/mL浓度范围内与峰面积呈良好的线性关系。在10~100 ng/g的浓度添加水平上，其回收率为73%~94%，批内、批间的相对标准偏差均小于12%。

Abstract:

A high-performance liquid chromatography(HPLC)-fluorescence detection method was developed for the determination of oxolinic acid and flumequine residues in eggs and milk. The samples were extracted with 1% formic acid in acetonitrile. The HPLC separation was carried out on a C18 column with 0.02 mol/L phosphoric acid-acetonitrile-tetrahydrofuran (68∶16∶16) as the mobile phase. A fluorescence detector was used at an excitation wavelength of 325 nm and an emission wavelength of 369 nm. A good linearity of the calibration curves for oxolinic acid and flumequine was obtained within the range of 3~500 ng/mL. Average recoveries of two drugs from egg and milk fortified at level of 10~100 ng/g were 73%~94%. The intra- and inter-batch variation coefficients were both less than 12%.