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QuEChERS-气相色谱质谱法快速测定水产品中扑草净残留

马丽莎 尹怡 田斐 谢文平 单奇 郑光明 李丽春 刘书贵 戴晓欣 赵城 魏琳婷 林嘉薇

马丽莎, 尹怡, 田斐, 谢文平, 单奇, 郑光明, 李丽春, 刘书贵, 戴晓欣, 赵城, 魏琳婷, 林嘉薇. QuEChERS-气相色谱质谱法快速测定水产品中扑草净残留[J]. 南方水产科学, 2022, 18(4): 170-176. doi: 10.12131/20210351
引用本文: 马丽莎, 尹怡, 田斐, 谢文平, 单奇, 郑光明, 李丽春, 刘书贵, 戴晓欣, 赵城, 魏琳婷, 林嘉薇. QuEChERS-气相色谱质谱法快速测定水产品中扑草净残留[J]. 南方水产科学, 2022, 18(4): 170-176. doi: 10.12131/20210351
MA Lisha, YIN Yi, TIAN Fei, XIE Wenping, SHAN Qi, ZHENG Guangming, LI Lichun, LIU Shugui, DAI Xiaoxin, ZHAO Cheng, WEI Linting, LIN Jiawei. Rapid determination of prometryn in aquatic products by QuEChERS combined with gas chromatography mass spectrometry[J]. South China Fisheries Science, 2022, 18(4): 170-176. doi: 10.12131/20210351
Citation: MA Lisha, YIN Yi, TIAN Fei, XIE Wenping, SHAN Qi, ZHENG Guangming, LI Lichun, LIU Shugui, DAI Xiaoxin, ZHAO Cheng, WEI Linting, LIN Jiawei. Rapid determination of prometryn in aquatic products by QuEChERS combined with gas chromatography mass spectrometry[J]. South China Fisheries Science, 2022, 18(4): 170-176. doi: 10.12131/20210351

QuEChERS-气相色谱质谱法快速测定水产品中扑草净残留

doi: 10.12131/20210351
基金项目: 中国-东盟海上合作基金 (CAMC-2018F);广东省渔业生态环境重点实验室开放基金 (FEEL-2020-8)
详细信息
    作者简介:

    马丽莎 (1981—),女,助理研究员,硕士,从事水产品质量安全与风险评估研究。E-mail: malisha16@163.com

    通讯作者:

    尹 怡 (1982—),女,副研究员,硕士,从事水产品质量安全与风险评估研究。E-mail: yin.yi@126.com

  • 中图分类号: TS 254.7

Rapid determination of prometryn in aquatic products by QuEChERS combined with gas chromatography mass spectrometry

  • 摘要: 以QuEChERS作为样品前处理手段,建立测定水产品中扑草净残留的气相色谱-质谱法 (GC-MS)。样品以乙腈-二氯甲烷 (VV=8∶2) 混合溶液提取,提取液经吸附剂中性氧化铝、N-丙基乙二胺 (PSA)、纳米二氧化锆结合石墨化炭黑 (GCB) 净化后上机检测,内标法定量。结果显示,扑草净质量浓度介于5~200 μg·L−1线性关系良好,相关系数 (R2) 为0.9999。对草鱼 (Ctenopharyngodon idellus)、鳜 (Siniperca chuatsi)、中国对虾 (Penaeus chinensis)、海参 (Holothuria sp.) 和文蛤 (Meretrix meretrix) 进行4个水平的加标回收实验 (10、20、40和200 µg·kg−1),方法的加标回收率为85.8%~111.8%,相对标准偏差为1.2%~8.8%,满足GB/T 27404—2008《实验室质量控制规范 食品理化检测》中实验室质量控制规范。扑草净的检出限 (LOD, S/N≥3) 和定量限 (LOQ, S/N≥10) 分别为5和10 µg·kg−1。该方法简单、快速、灵敏、净化效果好,能满足水产品中扑草净残留的检测需求。
  • 图  1  进样口不同温度对扑草净灵敏度的影响

    Figure  1.  Effect of different temperatures of injection port on sensitivity of prometryn

    图  2  不同提取溶剂提取效果的比较

    Figure  2.  Comparison of extraction effects of different extraction solvents

    图  3  不同提取溶剂对扑草净回收率的影响

    Figure  3.  Effects of differents extraction solvent on recoveries of prometryn

    图  4  3种吸附剂净化效果的比较

    Figure  4.  Comparison of purification effects of three adsorbents

    图  5  虾已净化与未净化基质的提取离子色谱图比较

    Figure  5.  Comparison of extracted ion diagrams of purified and unpurified shrimp

    图  6  僧帽牡蛎样品提取离子色谱图

    Figure  6.  Extracted ion chromatograms of S. cucullata

    表  1  水产品中扑草净的加标回收率和相对标准偏差 (N=6)

    Table  1.   Spiked recoveries and relative standard deviations of aquatic product (N=6)

    样品     
    Sample     
    回收率 Average recovery/% 相对标准偏差 RSD/%
    10 μg·kg−120 μg·kg−140 μg·kg−1200 μg·kg−1 10 μg·kg−120 μg·kg−140 μg·kg−1200 μg·kg−1
    海参 Holothuria sp. 107.2 97.2 94.2 103.9 8.3 4.5 4.3 3.1
    中国对虾 Penaeus chinensis 88.4 97.2 111.8 101.2 5.5 2.3 5.0 2.1
    草鱼 Ctenopharyngodon idellus 86.6 106.4 102.7 100.2 5.6 3.3 8.8 4.1
    Siniperca chuatsi 91.6 95.1 95.3 103.9 7.9 1.2 2.4 1.5
    文蛤 Meretrix meretrix 92.2 85.8 101.5 100.0 7.0 3.9 3.7 2.7
    下载: 导出CSV
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出版历程
  • 收稿日期:  2021-11-26
  • 修回日期:  2022-01-20
  • 录用日期:  2022-02-07
  • 网络出版日期:  2022-03-03
  • 刊出日期:  2022-08-05

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