柱前衍生化高效液相色谱一荧光检测法测定水产品中氨苄青霉素和阿莫西林残留

Determination of Ampicillin and Amoxicillin Residues in Aquatic Product Using Reversed-phase High Performance Liquid Chromatography-fluorescence Detection with Pre-column Derivatization

建立了柱前衍生化高效液相色谱一荧光检测法同时测定水产品中氨苄青霉素和阿莫西林含量。经固相萃取柱净化的样品通过衍生后，采用高效液相色谱荧光法测定。确定氨苄青霉素和阿莫西林线性范围为0．001-0．1mg／kg（r=0．9999），方法检出限分别为0．001mg／kg和0．005mg／kg（S／N=3），定量限分别为0．003mg／kg和0．015mg／kg（S／N=10），回收率为76．3％-96．8％，相对标准偏差（n=6）在0．63％-6．71％之间。该方法简便快速、结果准确，可作为测定水产品中氨苄青霉素和阿莫西林含量的有效方法。

A methd is developed for determination of ampicillin and amoxicillin residues in aquatic product using reversed-phase high performance liquid chromatography-fluorescence detection with pre-column derivatization. The sample extracts are cleaned up by solid-phase extraction cartridge and then derivatized with derivative agent. The results show that the calibration graphs is linear in the concentration rang of 0. 001 -0. 1 mg/kg（ r = 0. 999 9）. The detection limit and quantification limit are 0. 001 mg/kg（S/N =3） and 0. 003 mg/kg（S/N= 10） for ampicillin, O. 005 mg/kg（S/N=3） and 0. 015 mg/kg（ S/N= 10） for amoxicillin. The average recoveries are between 76. 3% -96. 8% with relative standard deviations （ RSDs ） of 0. 63 % - 6. 7 1% （ n = 6 ）. The method is simple, rapid, sensitive and reproducible, it can be used for the routine analysis of the ampicillin and amoxicillin residues in aquatic product.