QuEChERS试剂盒-高效液相色谱法检测鸡蛋中阿散酸和洛克沙砷残留

赵颖; 李典典; 张大卫; 魏月; 马晶军

doi:10.13386/j.issn1002-0306.2020050183

QuEChERS试剂盒-高效液相色谱法检测鸡蛋中阿散酸和洛克沙砷残留

Determination of Arsanilic acid and Roxarsone Residues in Eggs by QuEChERS kit -High Performance Liquid Chromatography

摘要

摘要: 建立QuEChERS试剂盒联用高效液相色谱检测鸡蛋中阿散酸和洛克沙砷的方法。样品经混匀后用乙腈与10%三氟乙酸的甲醇溶液（1:1，V/V）萃取，离心，取上清液于QuEChERS净化管（内含净化填料400 mg PSA、400 mg C₁₈EC、45 mg GCB、1199 mg MgSO₄）中净化萃取液，之后于高效液相色谱进行检测。结果表明，阿散酸和洛克沙砷在1.00～100.00 mg/L之间呈现良好线性关系，相关系数均大于0.999；方法检出限分别为0.044、0.063 mg/kg；定量限分别为0.149、0.211 mg/kg，阿散酸回收率在92.32%～95.95%，相对标准偏差1.54%～4.92%；洛克沙砷回收率是89.84%～94.91%，相对标准偏差2.19%～5.87%。本方法准确度高、精密度好、简便、快速，适用于鸡蛋中有机砷类兽药残留的检测，该研究为动物源性食品中禁用有机砷制剂的痕量分析奠定了方法基础。

Abstract: The method of using QuEChERS kit in combination with high performance liquid chromatography for determination of arsanilic acid and roxarsone in eggs was established. The sample was mixed and extracted with methanol solution (1:1, V/V) of acetonitrile and 10% trifluoroacetic acid, centrifuged, and the supernatant was taken and purified in QuEChERS purification tube (containing purification packing 400 mg PSA, 400 mg C₁₈EC, 45 mg GCB, 1199 mg MgSO₄), and then detected by HPLC.The results showed that there was a good linear relationship between arsanilic acid and roxarsone in the range of 1.00～100.00 mg/L, and the correlation coefficients were all greater than 0.999.The detection limits were 0.044 and 0.063 mg/kg, respectively.The quantitative limits were 0.149 and 0.211 mg/kg, respectively. The recovery rate of arsanilic acid was 92.32%～95.95%, and the relative standard deviation was 1.54%～4.92%. The recovery rate of roxarsone were 89.84%～94.91%, and the relative standard deviation was 2.19%～5.87%.The method has high accuracy, good precision, simple and rapid, and is suitable for the determination of organoarsenic veterinary drug residues in eggs.This study provides a method basis for trace analysis of banned organic arsenic preparations in animal-derived foods.