柱前衍生化高效液相色谱-荧光检测法测定水产品中氨苄青霉素和阿莫西林残留

摘要

A methd is developed for determination of ampicillin and amoxicillin residues in aquatic product using reversed-phase high performance liquid chromatography-fluorescenee 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(5/N = 3) and 0. 003 mg/kg(S/N= 10) for ampicillin, 0.005 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. 71% (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.%建立了柱前衍生化高效液相色谱-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0.001～0.1 mg/kg(r =0.999 9),方法检出限分别为0.001 mg/kg和0.005 mg/kg( S/N=3),定量限分别为0.003 mg/kg和0.015 mg/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.