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建立了柱前电化学氧化还原衍生-高效液相色谱测定鱼肉中结晶紫(CV)及隐性结晶紫(LCV)残留量的方法。试样用体积分数0.5%乙酸乙腈溶液提取,酸性氧化铝吸附剂净化,乙腈和乙酸铵缓冲液(78∶22,V/V)等度洗脱,柱前库仑检测器500 m V电压下LCV衍生为CV,588 nm波长检测。CV,LCV含量在0.010~0.50 mg/L范围内线性良好(γ>0.998),检出限为2.0μg/kg,定量限为5.0μg/kg。加标回收率为86.0%~91.0%。方法精密度、正确度和检出限等性能指标均达到兽残分析的要求,可用于水产品中CV,LCV测定。
A method for the determination of crystal violet (CV) and latent crystal violet (LCV) residues in fish meat by electrochemical redox-derivatization and high performance liquid chromatography was established. The sample was extracted with 0.5% acetic acid in acetonitrile, purified with acidic alumina adsorbent, isocratic eluted with acetonitrile and ammonium acetate buffer (78:22, V / V) and pre-column Coulometric detector at 500 mV Derived as CV, 588 nm wavelength detection. CV and LCV were linear in the range of 0.010-0.50 mg / L (γ> 0.998). The detection limit was 2.0 μg / kg and the limit of quantification was 5.0 μg / kg. Spike recovery was 86.0% ~ 91.0%. The method of precision, accuracy and detection limits and other performance indicators have reached the requirements of animal residue analysis can be used for determination of CV, LCV in aquatic products.