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QuEChERS-高效液相色谱-串联质谱法检测荔枝中氯虫苯甲酰胺、溴氰虫酰胺及代谢物残留

王思威 王潇楠 常虹 刘艳萍 孙海滨

王思威, 王潇楠, 常虹, 刘艳萍, 孙海滨. QuEChERS-高效液相色谱-串联质谱法检测荔枝中氯虫苯甲酰胺、溴氰虫酰胺及代谢物残留[J]. 农药学学报, 2022, 24(2): 395-403. doi: 10.16801/j.issn.1008-7303.2021.0177
引用本文: 王思威, 王潇楠, 常虹, 刘艳萍, 孙海滨. QuEChERS-高效液相色谱-串联质谱法检测荔枝中氯虫苯甲酰胺、溴氰虫酰胺及代谢物残留[J]. 农药学学报, 2022, 24(2): 395-403. doi: 10.16801/j.issn.1008-7303.2021.0177
WANG Siwei, WANG Xiaonan, CHANG Hong, LIU Yanping, SUN Haibin. Determination of chlorantraniliprole, cyantraniliprole and its metabolites residues in litchi using QuEChERS and high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Pesticide Science, 2022, 24(2): 395-403. doi: 10.16801/j.issn.1008-7303.2021.0177
Citation: WANG Siwei, WANG Xiaonan, CHANG Hong, LIU Yanping, SUN Haibin. Determination of chlorantraniliprole, cyantraniliprole and its metabolites residues in litchi using QuEChERS and high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Pesticide Science, 2022, 24(2): 395-403. doi: 10.16801/j.issn.1008-7303.2021.0177

QuEChERS-高效液相色谱-串联质谱法检测荔枝中氯虫苯甲酰胺、溴氰虫酰胺及代谢物残留

doi: 10.16801/j.issn.1008-7303.2021.0177
基金项目: 广州市科技计划项目(202102080338);广东省乡村振兴战略专项项目(403-2018-XMZC-0002-90);国家荔枝龙眼产业技术体系项目(CARS-32-15);广东省农业科学院院长基金项目(201929, 202026)
详细信息
    作者简介:

    王思威,344073564@qq.com

    通讯作者:

    刘艳萍,liuliuyp@tom.com

    孙海滨,sunhb@gdppri.cn.

  • 中图分类号: O657.63;TQ450.263

Determination of chlorantraniliprole, cyantraniliprole and its metabolites residues in litchi using QuEChERS and high performance liquid chromatography-tandem mass spectrometry

Funds: Guangzhou Science and Technology Project (202102080338), the Special Fund for Rural Revitalization Strategy of Guangdong Province (403-2018-XMZC-0002-90), China Agriculture Research System of MOF and MARA (CARS-32-15) and President Funding of Guangdong Academy of Agricultural Sciences (201929, 202026)
  • 摘要: 采用高效液相色谱-串联质谱(HPLC-MS/MS)技术,结合改良的QuEChERS法,建立了同时测定荔枝中氯虫苯甲酰胺、溴氰虫酰胺及代谢物J9Z38残留的分析方法。样品用乙腈提取,以N-丙基乙二胺(PSA)和十八烷基键合硅胶(C18)组合吸附剂净化,采用C18反相色谱柱分离,以V(甲酸水溶液) : V(乙腈)=15 : 85为流动相,采用电喷雾正离子扫描(ESI+),多反应监测(MRM)模式,外标法定量。结果表明:3种目标化合物在0.005~1 mg/L范围内线性关系良好(r>0.99);方法的定量限(LOQs)为0.0005~0.01 mg/kg;在0.0005~0.5 mg/kg添加水平下,氯虫苯甲酰胺、溴氰虫酰胺及代谢物在荔枝全果和果肉中的平均回收率为76%~98%,相对标准偏差(RSD)为2.5%~9.6%。应用该方法对广州市场中的20批次荔枝样品进行检测,结果显示,氯虫苯甲酰胺检出量为0.001~0.01 mg/kg,溴氰虫酰胺及其代谢物J9Z38未检出。该方法简便、高效、快速,可用于荔枝样品中双酰胺类农药的同时检测。
  • 图  1  3种提取溶剂对氯虫苯甲酰胺、溴氰虫酰胺及代谢物J9Z38的提取效率 (n=3)

    Figure  1.  Extraction rate of three extraction solvents for chlorantraniliprole, cyantraniliprole and its metabolite J9Z38 (n=3)

    图  2  5种吸附剂组合对氯虫苯甲酰胺、溴氰虫酰胺及代谢物J9Z38的吸附效率

    Figure  2.  Absorption efficiency of five adsorbent combinations for chlorantraniliprole, cyantraniliprole and its metabolite J9Z38

    图  3  不同色谱柱对氯虫苯甲酰胺、溴氰虫酰胺及代谢物J9Z38的分离效果 (0.05 mg/L)

    A: Agilent Infinity Lab Poroshell-120 SB-C18 (75 mm × 2.1 mm, 2.7 μm); B: Agilent Zorbax Extend-C18 (150 mm × 4.6 mm, 5.0 μm); C: Agilent Zorbax SB-Aq-C18 (150 mm × 4.6 mm, 5.0 μm); D: 岛津 Shim-pack GIST-HP C18 (100 mm × 2.1 mm, 3.0 μm); E: 岛津 Shim-pack GIST-HP C18 (150 mm × 2.1 mm, 3.0 μm).

    Figure  3.  Separation efficiency of different chromatographic columns for chlorantraniliprole, cyantraniliprole and its metabolite J9Z38 (0.05 mg/L)

    图  4  不同流动相对氯虫苯甲酰胺、溴氰虫酰胺及代谢物J9Z38的洗脱效果 (0.1 mg/L)

    Figure  4.  Elution effect of different mobile phase composition for chlorantraniliprole, cyantraniliprole and its metabolite J9Z38 (0.1 mg/L)

    图  5  氯虫苯甲酰胺(A)、溴氰虫酰胺 (B) 及代谢物J9Z38 (C) 的二级离子质谱图 (0.1 mg/L)

    Figure  5.  Mass spectrometry of product ions of chlorantraniliprole (A), cyantraniliprole (B) and its metabolite J9Z38 (C) (0.1 mg/L)

    表  1  氯虫苯甲酰胺、溴氰虫酰胺及代谢物J9Z38的质谱参数

    Table  1.   Mass spectra parameters of chlorantraniliprole, cyantraniliprole and its metabolite J9Z38

    化合物
    Compound
    母离子
    Precursor ion,
    m/z
    子离子
    Product ion,
    m/z
    碰撞能量
    Collision energy/
    V
    保留时间
    Retention time/
    min
    氯虫苯甲酰胺
    chlorantraniliprole
    484 285.9* −12 5.5
    453.35 −14
    溴氰虫酰胺
    cyantraniliprole
    475.3 285.95* −10 5.1
    444.1 −19
    代谢物J9Z38
    Metabolite J9Z38
    457.1 188* −27 6.3
    299 −35
    注(Note):*定量离子(Quantitative ion)。
    下载: 导出CSV

    表  2  吸附剂用量对氯虫苯甲酰胺、溴氰虫酰胺及代谢物J9Z38回收率的影响(n = 3)

    Table  2.   Effect of adsorbent dosage on the recovery of chlorantraniliprole, cyantraniliprole and its metabolite J9Z38 (n = 3)

    吸附剂组合
    Adsorbent combination
    回收率 Recovery/%
    代谢物J9Z38
    Metabolite J9Z38
    溴氰虫酰胺
    cyantraniliprole
    氯虫苯甲酰胺
    chlorantraniliprole
    MWCNT 5 mg 4±1.1 10±0.8 14±0.9
    MWCNT 10 mg 2±0.8 3±0.6 5±0.4
    PSA 50 mg + 5 mg GCB 16±2.4 32±1.0 43±1.6
    PSA 50 mg + 10 mg GCB 8±1.4 19±2.7 25±2.1
    PSA 50 mg + 20 mg GCB 5±2.9 12±5.0 18±7.1
    PSA 50 mg + C18 50 mg + 5 mg GCB 17±1.1 36±0.6 46±0.5
    PSA 50 mg + C18 50 mg + 10 mg GCB 9±1.6 19±1.7 29±2.6
    PSA 50 mg + C18 50 mg + 20 mg GCB 4±0.6 10±0.4 16±0.4
    PSA 25 mg + C18 25 mg + 5 mg GCB 28±2.6 31±3.8 45±1.4
    PSA 25 mg + C18 25 mg + 10 mg GCB 7±3.5 17±2.1 24±2.7
    C18 25 mg + 5 mg GCB 23±3.9 33±1.2 44±1.8
    C18 25 mg + 10 mg GCB 19±4.3 20±2.1 27±3.5
    PSA 25 mg + 5 mg GCB 15±2.0 34±1.4 44±4.2
    PSA 25 mg + 10 mg GCB 7±2.5 17±1.7 24±2.4
    PSA 100 mg + C18 50 mg 95±2.5 81±1.9 81±3.2
    PSA 50 mg + C18 100 mg 81±1.4 80±2.1 82±3.5
    PSA 50 mg + C18 50 mg 87±1.6 84±1.1 91±2.7
    注:表中数据为平均值 ± 标准差。Note: Data of the table are mean ± SD.
    下载: 导出CSV

    表  3  不同色谱柱下氯虫苯甲酰胺、溴氰虫酰胺及代谢物J9Z38线性方程及基质效应

    Table  3.   Linear equation and matrix effects of chlorantraniliprole, cyantraniliprole and its metabolite J9Z38 using different chromatographic columns

    色谱柱类型
    Chromatographic column
    化合物
    Compound
    基质
    Matrix
    线性方程
    Linear equation
    相关系数
    r
    基质效应
    Matrix effect/%
    A 氯虫苯甲酰胺 chlorantraniliprole 溶剂 Solvent y=1.56609 × 107x + 113324 0.9997
    果肉 Flesh y=1.36692 × 106x + 3949.26 0.9999 −91.3
    全果 Whole fruit y=1.16033 × 106x + 7783.01 0.9997 −92.6
    溴氰虫酰胺 cyantraniliprole 溶剂 Solvent y=5.25996 × 106x + 43758.2 0.9995
    果肉 Flesh y=151406x + 1780.56 0.9997 −97.1
    全果 Whole fruit y=148975x−1068.72 0.9979 −97.2
    代谢物 J9Z38 Metabolite J9Z38 溶剂 Solvent y=1.03342 × 106x−6121.65 0.9978
    果肉 Flesh y=577299x + 7626.68 0.9996 −44.1
    全果 Whole fruit y=392552x−3513.27 0.9971 −62.1
    B 氯虫苯甲酰胺 chlorantraniliprole 溶剂 Solvent y=1.15242 × 107x + 59844.7 0.9987
    果肉 Flesh y=1.22073 × 107x + 160325 0.9984 5.9
    全果 Whole fruit y=8.29595 × 106x + 144793 0.9992 −28.0
    溴氰虫酰胺 cyantraniliprole 溶剂 Solvent y=2.93376 × 106x + 15813.9 0.9988
    果肉 Flesh y=2.59718 × 106x + 35846.4 0.9981 −11.5
    全果 Whole fruit y=1.57836 × 106x + 18578.6 0.9988 −46.2
    代谢物 J9Z38 Metabolite J9Z38 溶剂 Solvent y=519147x + 2091.2 0.9994
    果肉 Flesh y=539501x + 4769.44 0.9994 3.9
    全果 Whole fruit y=176071x + 3453.94 0.9979 −66.1
    C 氯虫苯甲酰胺 chlorantraniliprole 溶剂 Solvent y=1.22326 × 107x + 66452.3 0.9999
    果肉 Flesh y=1.25802 × 107x + 270196 0.9963 2.8
    全果 Whole fruit y=8.05065 × 106x + 121095 0.9999 −34.1
    溴氰虫酰胺 cyantraniliprole 溶剂 Solvent y=4.30801 × 106x + 42111.2 0.9999
    果肉 Flesh y=3.33573 × 106x + 74203.7 0.9959 −22.6
    全果 Whole fruit y=2.32339 × 106x + 16241 0.9999 −46.1
    代谢物 J9Z38 Metabolite J9Z38 溶剂 Solvent y=645920x + 916.731 0.9999
    果肉 Flesh y=714497x + 16419.3 0.9959 10.6
    全果 Whole fruit y=424131x + 3202.63 0.9999 −34.3
    注 (Note): A: Agilent Infinity Lab Poroshell-120 SB-C18 (75 mm × 2.1 mm, 2.7 μm); B: Agilent Zorbax Extend-C18 (150 mm × 4.6 mm, 5.0 μm); C: Agilent Zorbax SB-Aq-C18 (150 mm × 4.6 mm, 5.0 μm).
    下载: 导出CSV

    表  4  氯虫苯甲酰胺、溴氰虫酰胺及代谢物J9Z38在荔枝中的添加回收率、相对标准偏差及定量限 (n=5)

    Table  4.   Recoveries, RSDs, and LOQ of chlorantraniliprole, cyantraniliprole and its metabolite J9Z38 in litchi pulp and whole fruits (n=5)

    化合物
    Compound
    基质
    Matrix
    添加水平
    Spiked
    level/
    (mg/kg)
    回收率
    Recoveries/
    %
    相对
    标准偏差
    RSD/
    %
    定量限
    LOQ/
    (mg/kg)
    氯虫苯甲酰胺
    chlorantraniliprole
    果肉
    Flesh
    0.0005 80 4.7 0.0005
    0.01 87 8.6
    0.1 96 5.8
    0.5 97 5.4
    全果
    Whole fruit
    0.0005 78 8.1 0.0005
    0.01 96 6.7
    0.1 93 5.3
    0.5 84 5.0
    溴氰虫酰胺
    cyantraniliprole
    果肉
    Flesh
    0.005 78 5.1 0.005
    0.01 88 5.6
    0.1 98 3.9
    0.5 91 3.5
    全果
    Whole fruit
    0.005 76 7.3 0.005
    0.01 92 8.5
    0.1 95 5.1
    0.5 81 2.5
    代谢物J9Z38
    Metabolite J9Z38
    果肉
    Flesh
    0.01 88 6.4 0.01
    0.1 95 5.6
    0.5 92 6.0
    全果
    Whole fruit
    0.01 95 9.6 0.01
    0.1 92 8.1
    0.5 86 6.8
    下载: 导出CSV
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出版历程
  • 收稿日期:  2021-07-08
  • 录用日期:  2021-11-12
  • 网络出版日期:  2021-12-27
  • 刊出日期:  2022-04-01

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