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目的建立QuEChERS净化—超高效液相色谱法测定淡水鱼中孔雀石绿、结晶紫及其代谢物的方法。方法样品经QuEChERS方法前处理,采用ZORBAX Extend C18(2.1 mm i.d×50 mm,1.8μm)分离,以乙腈乙酸铵缓冲液梯度洗脱,流速为0.5 ml/min,二极管阵列检测器检测孔雀石绿(λ=620 nm)及结晶紫(λ=588 nm),荧光检测隐性孔雀石绿与隐性结晶紫(激发波长:265 nm,发射波长360 nm)。结果孔雀石绿与结晶紫在10μg/L~200μg/L,隐色孔雀石绿、隐性结晶紫在2.0μg/L~40μg/L范围内有良好的线性关系(r>0.999),检测限为0.36μg/kg~5.1μg/kg,平均加标回收率为69%~118%,相对标准偏差1.8%~10%。结论方法快速、简单,可应用于淡水鱼中孔雀石绿、结晶紫及其代谢物残留量的检测。
Objective To establish a method for the determination of malachite green, crystal violet and its metabolites in freshwater fish by QuEChERS purification - ultra performance liquid chromatography. Methods The samples were pretreated by QuEChERS method and separated by ZORBAX Extend C18 (2.1 mm id × 50 mm, 1.8 μm). The gradient was eluted with acetonitrile-ammonium acetate buffer at a flow rate of 0.5 ml / min. The malachite green (λ = 620 nm) and crystal violet (λ = 588 nm). The fluorescence of latent malachite green and latent crystal violet (excitation wavelength: 265 nm, emission wavelength: 360 nm) were detected. Results There was a good linear relationship between malachite green and crystal violet in the range of 10μg / L ~ 200μg / L, leucomalachite green and latent crystal violet in the range of 2.0μg / L ~ 40μg / L (r> 0.999) 0.36μg / kg ~ 5.1μg / kg, the average recovery was 69% ~ 118%, the relative standard deviation of 1.8% to 10%. Conclusion The method is rapid and simple and can be applied to the detection of malachite green, crystal violet and its metabolites in freshwater fish.