摘要
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 A method was developed for the determination of malachite green (MG) and crystal violet (CV) and their major metabolite, leucomalachite green (LMG) and leueinecrystal violet (LCV) , in freshwater fish by Ultra High Per- formance Liquid Chromatography (UHPLC) using QuEChERS approach. Methods Sample was extracted and cleaned up using QuEChERS approach. UHPLC separation was achieved by using ZORBAX Extend Cls (2.1 mm i. d × 50 mm, 1.8μm) with an mobile phase consisting of acetonitrile and acetate buffer and gradient program was used at a flow rate of 0.5 ml/min. DAD de- tector was used for the determination of MG (A = 620 nm) and CV (A = 588 nm) , while LMG and LCV were detected by fluo- rescence detector (Aex = 265 nm and A em = 360 nm). Results Calibration curves have a good linear relationship (r 〉 0.999) in the range of 10μg/L× 200 μg,/L for MG and CV, while 2.0 μg/L N 40μg/L for LMG and LCV . The limits of detection (LOD) were from 0.36μg/kg to 5.1μg/kg respectively. The average recoveries were from 69% to 118%, with relative stand- ard deviations (RSDs) from 1.8% to 10%. Conclusion The method is simple, rapid and could be applied for the analysis of MG, CV and their metabolite in freshwater fish.
出处
《中国卫生检验杂志》
北大核心
2013年第11期2445-2447,2452,共4页
Chinese Journal of Health Laboratory Technology
关键词
QUECHERS
超高效液相色谱
孔雀石绿
隐性孔雀石绿
结晶紫
隐性结晶紫
残留分析
QuEChERS
Ultra high performance liquid chromatography (UHPLC)
Malachite green
Leucomalachite green
Crystal violet
Leucineerystal violet
Residues analysis