用高效液相色谱法检测水产品中磺胺类、乙胺嘧啶等合成抗菌剂残留.样品以乙腈、二氯甲烷、乙酸乙酯以体积比2比1比1为提取剂,经脱脂、净化、浓缩,用流动相溶解.用高效液相色谱法紫外检测器测定.通过梯度洗脱将7种磺胺类、乙胺嘧啶进行分离.各标准曲线线性范围为0.05~2.0 mg·L-1,相关系数为0.983 7~0.997 5,回收率分别为62.2%~88.6%,相对标准偏差为5.85%~8.12%(n=7),检出限(S/N=3)为10~50 μg·kg-1.

HPLC was applied to the determination of residual sulfanilamides and ethylaminopyrimidines in aquatic products.The residual drugs in the sample were extracted with a solvent mixture of acetonitrile,dichloromethan and ethyl acetate mixed in the proportion of 2∶1∶1 respectively.The extract obtained was defatted and purified by extraction with hexane,and the hexane extract was then concentrated by evaporation.The residue was taken up with a mixed solvent of acetonitrile,acetic acid(2+98) and H2O mixed in the ratio of 15+25+60,which was used also as the mobile phase in the chromatographic separation later.Seven kinds of sulfanilamide and ethylaminopyrimidine drugs were well separated by gradient elution on the chromatographic column of Clovisl-C18(4.6 mm×150 mm,5 μm),and their contents determined by UV-detection at the wavelength of 275 nm.Linear relationship between the peak area and the concentration of standards of the 7 different drugs were found all in range of 0.05-2.0 mg·L-1,with correlation coefficients in the range of 0.983 7 to 0.997 5.In the tests for precision,accuracy and sensitivity of the proposed method,the results obtained were as follows: RSD′s 5.85%-8.12%,recovery 62.2%-88.6%,detection limit(S/N=3) 10-50 μg·kg-1.