高效液相色谱法测定欧洲鳗鲡肌肉中磺胺嘧啶和磺胺甲噁唑残留
Simultaneous Determination of Sulfadiazine and Sulfamethoxazole Residues in Muscle of European Eels (Anguilla anguilla)by HPLC
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摘要: 建立了欧洲鳗鲡肌肉中磺胺嘧啶和磺胺甲噁唑的高效液相色谱检测方法。均质肌肉样品采用乙腈∶氯仿(10∶1)提取,提取液经氮吹浓缩,残渣用2 mL流动相溶解,饱和正己烷脱脂净化,采用Eclipse XDB-C18 色谱柱,以乙腈∶0.05 molL-1磷酸二氢铵(20∶80)为流动相, 多波长紫外检测器检测。磺胺嘧啶和磺胺甲噁唑的检出限分别为4、8 gkg-1,在0.01~5.0 gg-1添加范围内,平均回收率均大于80%,日内与日间RSD均小于5%,说明方法满足常规残留检测要求。Abstract: A high performance liquid chromatographic method was developed for the simultaneous determination of sulfadiazine and sulfamethoxazole in European eels (Anguilla anguilla) muscle. Homogenized tissue were extracted with 10% sodium sulfate and acetonitrile- Chloroform(10∶1), the extract was concentrated by nitrogen, and redissolved into 2 mL mobile phase and defatted with n-hexane. Sulfadiazine and sulfamethoxazole were separated on Eclipse XDB-C18 Column with mobile phases containing acetonitrile and 0.05 molL-1 ammonium dihydrogen phosphate (20∶80) and finally determined by Multiple Wavelength Detector (MWD). The detection limit of sulfadiazine and sulfamethoxazole were 4 gkg-1and 8 gkg-1.In the range of 0.01~5.0 gkg-1, the mean recoveries were more than 80%. The intraday and interday precisions were less than 5%. It showed that the method meet the conventional residue testing requirements.