QuEChERS UHPLC测定淡水鱼中孔雀石绿结晶紫及其代谢物  

Determination of malachite green,crystal violet and their metabolite residues in freshwater fish by ultra high performance liquid chromatography using QuEChERS approach

作　　者：欧阳燕玲[1] 谢维平[1] 苏碧玲[1] 

机构地区：[1]泉州市疾病预防控制中心,福建泉州362000

出　　处：《中国卫生检验杂志》2013年第11期2445-2447,2452,共4页Chinese Journal of Health Laboratory Technology

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.

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 

分 类 号：O657.72[理学—分析化学]