HPLC Determination of Residual Sulfanilamides and Ethylaminopyrimidines in Aquatic Products
標 簽 高效液相色譜 磺胺類 乙胺嘧啶 High performance liquid chromatography Sulfanilamides Ethylaminopyrimidines
用高效液相色譜法檢測水產品中磺胺類、乙胺嘧啶等合成抗菌劑殘留.樣品以乙腈、二氯甲烷、乙酸乙酯以體積比2比1比1為提取劑,經脫脂、凈化、濃縮,用流動相溶解.用高效液相色譜法紫外檢測器測定.通過梯度洗脫將7種磺胺類、乙胺嘧啶進行分離.各標準曲線線性范圍為0.05~2.0 mg·L-1,相關系數為0.983 7~0.997 5,回收率分別為62.2%~88.6%,相對標準偏差為5.85%~8.12%(n=7),檢出限(S/N=3)為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.
引用該論文: LI Zuo-qing,NI Mei-lin,ZHANG Zai-ting,XIE Dong-hua,YU Xue-jun,ZHAN Jia,YIN Ju-yi. HPLC Determination of Residual Sulfanilamides and Ethylaminopyrimidines in Aquatic Products[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2008, 44(6): 557～559
李佐卿,倪梅林,章再婷,謝東華,俞雪鈞,湛嘉,殷居易. 高效液相色譜法檢測水產品中磺胺類和乙胺嘧啶藥物殘留[J]. 理化檢驗－化學分冊, 2008, 44(6): 557～559
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