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

赵颖,李典典,张大卫,等. 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[J]. 食品工业科技,2021,42(7):252−257. doi:  10.13386/j.issn1002-0306.2020050183
引用本文: 赵颖,李典典,张大卫,等. 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[J]. 食品工业科技,2021,42(7):252−257. doi:  10.13386/j.issn1002-0306.2020050183
ZHAO Ying, LI Diandian, ZHANG Dawei, et al. Determination of Arsanilic acid and Roxarsone Residues in Eggs by QuEChERS kit -High Performance Liquid Chromatography [J]. Science and Technology of Food Industry, 2021, 42(7): 252−257. (in Chinese with English abstract). doi:  10.13386/j.issn1002-0306.2020050183
Citation: ZHAO Ying, LI Diandian, ZHANG Dawei, et al. Determination of Arsanilic acid and Roxarsone Residues in Eggs by QuEChERS kit -High Performance Liquid Chromatography [J]. Science and Technology of Food Industry, 2021, 42(7): 252−257. (in Chinese with English abstract). 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

doi: 10.13386/j.issn1002-0306.2020050183
基金项目: 河北省科技计划项目“河北省山区特色杂果近自然生产技术及产品加工创新与示范”(16236802D-14);河北农业大学师生协同创新项目“葡萄浓缩汁去除酒石酸加工关键技术研究”(bhxt201813)
详细信息
    作者简介:

    赵颖(1998−),女,本科,研究方向:食品质量与安全,E-mail:zhaoying1416@sina.com

    通讯作者:

    魏月(1989−),女,硕士,讲师,研究方向:食品质量与安全,E-mail:weiyueyueyue@sina.com

    马晶军(1971−),男,硕士,教授,研究方向:分析化学研究,E-mail:mjjwjpmartin@sina.com

  • 中图分类号: TS207.3

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

  • 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 C18 EC、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。
  • 图  1  三种前处理条件下不同净化填料的比较

    Figure  1.  Comparison of different purification fillers under three pretreatment conditions

    图  2  在相同试验条件下萃取剂浓度对回收率的影响

    Figure  2.  Effect of extractant concentration on the recovery under the same experimental conditions

    图  3  相同试验条件下萃取剂比例对回收率的影响

    Figure  3.  Effect of extractant in different proportions on the recovery under the same experimental conditions

    图  4  加标鸡蛋样品的HPLC图

    Figure  4.  HPLC diagram of standard egg sample

    表  1  不同方法灵敏度的比较

    Table  1.   Sensitivity comparison of different methods

    前处理方法样品加标浓度ASA ROX参考文献
    LOD加标回收率(%)RSD(%)LOD加标回收率(%)RSD(%)
    QuEChERS鸡蛋1 mg/L0.044 mg/kg92.321.540.063 mg/kg90.162.19
    固相萃取技术饲料20 μg/g0.095 mg/kg88.66.20.19 mg/kg86.04.7[9]
    加速溶剂萃取法猪肝0.5 mg/kg2.4 μg/L92.24.64.1 μg/L89.33.9[12]
    微波辅助萃取法鸡蛋0.1 mg/kg0.1 mg/kg83.53.40.2 mg/kg84.51.81[20]
    下载: 导出CSV

    表  2  样品加标回收率及精密度

    Table  2.   Recovery and precision of standardized samples

    化合物加标浓度(mg/L)加标回收率(%)相对标准偏差(%)
    ASA1.0092.321.54
    50.0095.134.63
    100.0095.954.92
    ROX1.0090.162.19
    50.0089.845.87
    100.0094.914.73
    下载: 导出CSV

    表  3  实际样品测定(mg/kg)

    Table  3.   Actual sample determination(mg/kg)

    样品ASA含量ROX含量样品ASA含量ROX含量
    柴鸡蛋1NDND普通鸡蛋1NDND
    柴鸡蛋2NDND普通鸡蛋2NDND
    柴鸡蛋3NDND普通鸡蛋3NDND
    柴鸡蛋4NDND普通鸡蛋4NDND
    注:“ND”表示未检出。
    下载: 导出CSV
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出版历程
  • 收稿日期:  2020-05-18
  • 网络出版日期:  2021-01-28
  • 刊出日期:  2021-04-01

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