同位素稀释-高效液相色谱-高分辨质谱法测定乳及乳制品中3种三嗪类农药

李巧 戴唯 王缅 朱明

李巧,戴唯,王缅,等. 同位素稀释-高效液相色谱-高分辨质谱法测定乳及乳制品中3种三嗪类农药[J]. 食品工业科技,2021,42(21):263−271. doi:  10.13386/j.issn1002-0306.2021010032
引用本文: 李巧,戴唯,王缅,等. 同位素稀释-高效液相色谱-高分辨质谱法测定乳及乳制品中3种三嗪类农药[J]. 食品工业科技,2021,42(21):263−271. doi:  10.13386/j.issn1002-0306.2021010032
LI Qiao, DAI Wei, WANG Mian, et al. Determination of Three Triazine Pesticides in Milk and Dairy Products by Isotope Dilution-High Performance Liquid Chromatography-High Resolution Mass Spectrometry[J]. Science and Technology of Food Industry, 2021, 42(21): 263−271. (in Chinese with English abstract). doi:  10.13386/j.issn1002-0306.2021010032
Citation: LI Qiao, DAI Wei, WANG Mian, et al. Determination of Three Triazine Pesticides in Milk and Dairy Products by Isotope Dilution-High Performance Liquid Chromatography-High Resolution Mass Spectrometry[J]. Science and Technology of Food Industry, 2021, 42(21): 263−271. (in Chinese with English abstract). doi:  10.13386/j.issn1002-0306.2021010032

同位素稀释-高效液相色谱-高分辨质谱法测定乳及乳制品中3种三嗪类农药

doi: 10.13386/j.issn1002-0306.2021010032
基金项目: 法规差异性化学有害物精准侦查技术研究(2017YFC1601603)
详细信息
    作者简介:

    李巧(1995−),女,本科,助理工程师,研究方向:食品理化检验,E-mail:406873130@qq.com

    通讯作者:

    朱明(1979−),男,硕士研究生,工程师,研究方向:食品理化检验,E-mail:butterflymz@126.com

  • 中图分类号: TS252.7

Determination of Three Triazine Pesticides in Milk and Dairy Products by Isotope Dilution-High Performance Liquid Chromatography-High Resolution Mass Spectrometry

  • 摘要: 本文建立了乳及乳制品中莠去津、灭蝇胺和异丙甲草胺3种三嗪类农药残留的同位素稀释-高效液相色谱-高分辨质谱的测定方法。样品采用乙腈提取,经C18固相萃取小柱净化后测定。以甲醇-0.1%甲酸水溶液为流动相梯度洗脱,待测物经Hypersil GOLD C18色谱柱分离,最后用电喷雾正离子(HESI+)和全扫描/数据依赖二级扫描(Full MS/dd-MS2)模式进行定性定量检测。结果表明:3种三嗪类农药在1.0~50.0 ng/mL浓度范围内线性关系良好(r2≥0.99)。方法检出限为5 μg/kg,添加水平为5、10、25 μg/kg时,平均回收率为81.6%~104.0%,相对标准偏差为0.55%~4.14%。该方法适用于乳及乳制品中3种三嗪类农药残留的检测,灵敏度高、重现性好、结果可靠,为保障我国乳及乳制品的食品安全提供了技术支撑。
  • 图  1  3种三嗪类农药的色谱峰及离子碎片图

    Figure  1.  Chromatographic peaks and ion fragment profiles of three triazines

    图  2  不同流动相对3种三嗪类农药响应值的影响

    Figure  2.  The effects of different types of the mobile phase on response values of three triazine pesticides

    图  3  不同色谱柱对3种三嗪类农药响应值的影响

    Figure  3.  Effect of different chromatographic columns on response values of three triazine pesticides

    图  4  不同提取剂对莠去津的影响

    Figure  4.  Effects of different solvents on atrazine

    图  5  不同提取剂对灭蝇胺的影响

    Figure  5.  Effects of different solvents on cyromazine

    图  6  不同提取剂对异丙甲草胺的影响

    Figure  6.  Effects of different solvents on metolachlor

    图  7  不同净化柱对3种三嗪类农药的影响

    Figure  7.  Effects of different purification columns on three triazine pesticides

    表  1  3种三嗪类农药及其内标分子式、保留时间、母离子、离子碎片、结构式

    Table  1.   Three kinds of triazine pesticides and their internal molecular formula, retention time, parent ion, ion fragment and structural formula

    化合物分子式保留时间(min)母离子(m/z)碎片离子(m/z)结构式
    异丙甲草胺C8H14ClN58.33284.14118252.11403
    异丙甲草胺-D6C15H16ClD6NO28.34290.17813Lock Masses
    灭蝇胺C6H10N60.90167.1039785.05158
    灭蝇胺-13C3C313C3H10N60.91170.11389Lock Masses
    莠去津C8H14ClN57.60216.10105174.05426
    莠去津-D5C8H9ClD5N57.59221.13206Lock Masses
    下载: 导出CSV

    表  2  内标法和外标法差异比较

    Table  2.   Comparison between internal standard method and external standard method

    目标物外标法内标法
    添加水平(μg/kg)回收率(%)添加水平(μg/kg)回收率(%)
    灭蝇胺25.069.425.089.7
    莠去津25.091.125.098.6
    异丙甲草胺25.089.225.093.7
    下载: 导出CSV

    表  3  3种三嗪类农药的线性回归方程、相关系数、回收率和相对标准偏差(n=6)

    Table  3.   Linear equations, correlation coefficients, standard recoveries and relative standard deviations of three triazine pesticides(n=6)

    目标化合物线性回归方程相关系数(r2样品名称5 μg/kg10 μg/kg25 μg/kg
    平均回收率(%)RSD(%)平均回收率(%)RSD(%)平均回收率(%)RSD(%)
    灭蝇胺Y=-0.516872X0.9989牛奶84.502.3789.601.4590.000.90
    奶粉87.204.1291.202.9181.603.22
    酸奶92.803.3288.103.1093.302.73
    莠去津Y=0.467975X0.9997牛奶94.900.5598.600.7997.601.28
    奶粉100.001.76104.001.49102.001.19
    酸奶98.400.9199.700.87100.001.03
    异丙甲草胺Y=0.578078X0.9989牛奶88.901.6393.701.4793.801.84
    奶粉94.304.1499.502.43101.001.72
    酸奶92.202.6294.001.2795.200.86
    下载: 导出CSV
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出版历程
  • 收稿日期:  2021-01-09
  • 网络出版日期:  2021-09-14

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    《食品工业科技》编辑部携手万方数据开通学术不端专属检测通道,具体信息参见本刊动态。