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6类茶叶中15种农药残留过程中产生的基质效应研究

陈璐 李怀平 王顾希 唐祥凯 冯德建 魏雨婷

陈璐,李怀平,王顾希,等. 6类茶叶中15种农药残留过程中产生的基质效应研究 [J]. 福建农业学报,2024,39(6):720−728
引用本文: 陈璐,李怀平,王顾希,等. 6类茶叶中15种农药残留过程中产生的基质效应研究 [J]. 福建农业学报,2024,39(6):720−728
CHEN L, LI H P, WANG G X, et al. Study on matrix effects in the detection of 15 pesticide residues in 6 types of tea leaves [J]. Fujian Journal of Agricultural Sciences,2024,39(6):720−728
Citation: CHEN L, LI H P, WANG G X, et al. Study on matrix effects in the detection of 15 pesticide residues in 6 types of tea leaves [J]. Fujian Journal of Agricultural Sciences,2024,39(6):720−728

6类茶叶中15种农药残留过程中产生的基质效应研究

基金项目: 四川省重点研发计划项目(2020YFN0003、2020YFN0154);四川省自然科学基金项目(2022NSFSC1775)
详细信息
    作者简介:

    陈璐(1991 — ),女,工程师,主要从事食品质量安全研究,E-mail:165374435@qq.com

    通讯作者:

    唐祥凯(1986 — ),男,硕士研究生,副研究员,主要从事食品质量安全研究,E-mail:460427982@qq.com

  • 中图分类号: TS272

Study on matrix effects in the detection of 15 pesticide residues in 6 types of tea leaves

  • 摘要:   目的  对气相色谱-串联质谱法测定6类茶叶中15种农药残留过程中产生的基质效应进行分析,并就日常检测中常见批量样品同时处理时可采用的替代基质进行探讨。   方法  茶叶样品经QuEChERS前处理,配制质量浓度在0.01~0.32 mg·L−1的溶剂标准曲线和基质标准曲线,经GC-MS/MS测定后计算基质效应。  结果  6类茶叶中15种农药检测过程中均产生增强基质效应,其中以增强强基质效应为主,基质效应区间范围1.35%~411.58%, 强、中、弱基质效应分别为73.33%、23.33%、3.33%。以红茶为替代基质测定15种农药时,主要以产生增强弱基质效应为主,整体区间范围为|0.62%|~|59.22%|,强中弱基质效应分别为1.33%、14.67%、84.00%;以混合茶叶为代表基质测定15种农药时,主要以产生抑制弱基质效应为主,整体区间范围为|0.09%|~|48.09%|,强中弱基质效应分别为0、13.33%、86.67%。  结论  茶叶样品基质复杂,在农残检测时使用基质标曲分析可降低基质效应,提高检测结果的准确度。使用混合茶叶样品作为替代基质配制基质标曲对茶叶农残进行定量分析时,可有效提高批量样品的分析效率。
  • 图  1  15种农药典型MRM色谱图

    1. 敌敌畏;2.甲拌磷;3.五氯硝基苯;4.毒死蜱;5.马拉硫磷; 6.杀螟硫磷;7.甲基异柳磷; 8.水胺硫磷;9.腐霉利;10.杀扑磷; 11.联苯菊酯;12.甲氰菊酯;13.氯菊酯;14.溴氰菊酯;15.苯醚甲环唑。

    Figure  1.  Typical MRM chromatogram of 15 pesticide residues

    1: dichlorvos; 2: phorate; 3: pentachloronitrobenzene; 4: chlorpyrifos; 5: malathion; 6: fenitrothion; 7: isofenphos-methy; 8: isocarbophos; 9: procymidone; 10: methidathion; 11: bifenthrin; 12: fenpropathrin; 13: permethrin; 14: deltamethrin; 15: difenoconazole.

    图  2  以红茶为代表基质矫正后5类茶叶中15种农药检测过程中产生的基质效应占比

    Figure  2.  Proportion of matrix effects generated in detecting 15 pesticides in 5 types of tea with black tea used as a representative matrix

    图  3  以混合茶为代表基质矫正后6类茶叶中15种农药检测过程中产生的基质效应占比

    Figure  3.  Proportion of matrix effects generated in detecting 15 pesticides in 6 types of tea with mixed tea used as a representative matrix

    表  1  15种农药名称、CAS号、色谱及质谱参数及定量限

    Table  1.   Chemical abstract service(CAS) number,GC-MS/MS parameters and limit of quantitation of 15 pesticide residues

    序号
    No.
    目标物
    Compound
    CAS号
    CAS
    number
    保留时间
    Retention
    time/min
    母离子
    Precursor
    ions(m/z)
    子离子
    Product
    ions(m/z)
    碰撞能量
    Collision
    energy/eV
    定量限
    limit of quantitation/
    (mg·kg−1
    线性范围
    Linear range/
    (mg·kg−1
    1 敌敌畏 Dichlorvos 62-73-7 6.81 109.0 79.0* 5 0.05 0.01~0.32
    184.9 93.0 10
    2 甲拌磷 Phorate 298-02-2 14.17 260.0 75.0* 5 0.01 0.01~0.32
    230.9 128.9 25
    3 五氯硝基苯 Pentachloronitrobenzene 82-68-8 15.32 295.0 237.0* 20 0.05 0.01~0.32
    236.9 142.9 30
    4 毒死蜱 Chlorpyrifos 2921-88-2 19.73 196.9 169.0* 15 0.05 0.01~0.32
    198.9 171.0 15
    5 马拉硫磷 Malathion 121-75-5 20.39 126.9 99.0* 5 0.05 0.01~0.32
    172.9 99.0 15
    6 杀螟硫磷 Fenitrothion 122-14-5 20.42 277.0 260.0* 5 0.05 0.01~0.32
    277.0 109 20
    7 甲基异柳磷 Isofenphos-methy 99675-03-3 21.44 199.0 121.0* 10 0.01 0.01~0.32
    241.1 199.1 10
    8 水胺硫磷 Isocarbophos 24353-61-5 21.74 135.9 108.0* 15 0.05 0.01~0.32
    135.9 69.0 30
    9 腐霉利 Procymidone 32809-16-8 23.10 96.0 67.1* 10 0.05 0.01~0.32
    96.0 53.1 15
    10 杀扑磷 Methidathion 950-37-8 23.11 144.9 85.0* 5 0.05 0.01~0.32
    144.9 58.1 15
    11 联苯菊酯 Bifenthrin 82657-04-3 27.35 181.2 165.2* 25 0.05 0.01~0.32
    181.2 166.2 10
    12 甲氰菊酯 Fenpropathrin 39515-41-8 28.34 207.9 181.0* 5 0.05 0.01~0.32
    264.9 210.0 10
    13 氯菊酯 Permethrin 51877-74-8 29.97 183.1 168.1* 10 0.05 0.01~0.32
    183.1 153.0 15
    14 溴氰菊酯 Deltamethrin 52918-63-5 33.13 252.9 93.0* 15 0.05 0.01~0.32
    250.7 172.0 5
    15 苯醚甲环唑 Difenoconazole 119446-68-3 33.25 322.8 264.8* 15 0.05 0.01~0.32
    264.9 202.0 20
    *定量离子对。
    *: quantitative ion.
    下载: 导出CSV

    表  2  6类茶叶中15种农药检测过程中产生的基质效应比较

    Table  2.   Matrix effects generated in detecting 15 pesticide residues in 6 types of tea

    农药名称
    Pesticide name
    基质效应 ME/%
    绿茶
    Green tea
    红茶
    Black tea
    花茶
    Scented tea
    黑茶
    Dark tea
    白茶
    White tea
    乌龙茶
    Oolong
    绝对平均值
    Absolute mean
    敌敌畏 Dichlorvos 1.35 31.59 8.81 27.06 35.20 38.15 23.69
    甲拌磷 Phorate 6.13 43.31 23.75 72.32 56.16 60.19 43.64
    五氯硝基苯 Pentachloronitrobenzene 47.35 23.34 45.46 39.95 48.73 60.08 44.15
    毒死蜱 Chlorpyrifos 57.39 48.00 56.25 33.78 66.10 75.31 56.14
    马拉硫磷 Malathion 101.11 148.50 123.92 154.93 161.75 153.84 140.68
    杀螟硫磷 Fenitrothion 112.99 135.59 126.29 145.96 134.13 156.16 135.19
    甲基异柳磷 Isofenphos-methy 66.55 44.65 60.34 61.92 64.59 70.01 61.34
    水胺硫磷 Isocarbophos 108.10 140.04 115.11 152.66 158.59 178.60 142.18
    腐霉利 Procymidone 57.67 34.95 53.11 73.39 55.28 61.84 56.04
    杀扑磷 Methidathion 14.51 180.82 58.92 142.15 138.94 104.98 106.72
    联苯菊酯 Bifenthrin 39.66 30.69 40.75 50.40 48.68 50.76 43.49
    甲氰菊酯 Fenpropathrin 76.60 75.33 81.19 95.37 94.99 88.00 85.25
    氯菊酯 Permethrin 85.72 79.55 83.41 110.82 103.12 107.78 95.07
    溴氰菊酯 Deltamethrin 269.31 298.67 304.64 394.83 354.78 366.68 331.49
    苯醚甲环唑 Difenoconazole 211.21 391.51 279.99 411.58 344.98 381.49 336.79
    下载: 导出CSV

    表  3  以红茶为代表基质时5类茶叶中15种农药检测过程中产生的基质效应比较

    Table  3.   Matrix effects generated in detecting 15 pesticides in 5 types of tea with black tea used as a representative matrix

    农药名称
    Pesticide name
    基质效应 ME/%
    绿茶
    Green tea
    花茶
    Scented tea
    黑茶
    Dark tea
    白茶
    White tea
    乌龙茶
    Oolong
    绝对平均值
    Absolute mean
    敌敌畏 Dichlorvos −22.98 −17.31 −3.45 2.75 4.99 10.29
    甲拌磷 Phorate −25.95 −13.65 20.24 8.96 11.78 16.12
    五氯硝基苯 Pentachloronitrobenzene 19.47 17.93 13.46 20.58 29.79 20.25
    毒死蜱 Chlorpyrifos 6.34 5.58 −9.61 12.23 18.45 10.44
    马拉硫磷 Malathion −19.07 −9.89 2.59 5.33 2.15 7.81
    杀螟硫磷 Fenitrothion −9.59 −3.95 4.40 −0.62 8.73 5.46
    甲基异柳磷 Isofenphos-methy 15.14 10.84 11.93 13.78 17.53 13.85
    水胺硫磷 Isocarbophos −13.30 −10.39 5.26 7.73 16.07 10.55
    腐霉利 Procymidone 16.83 13.45 28.48 15.07 19.93 18.75
    杀扑磷 Methidathion −59.22 −43.41 −13.77 −14.91 −27.01 31.66
    联苯菊酯 Bifenthrin 6.87 7.70 15.09 13.76 15.36 11.75
    甲氰菊酯 Fenpropathrin 0.73 3.34 11.43 11.22 7.23 6.79
    氯菊酯 Permethrin 3.44 2.15 17.42 13.13 15.73 10.37
    溴氰菊酯 Deltamethrin −7.37 1.50 24.12 14.07 17.06 12.82
    苯醚甲环唑 Difenoconazole −36.68 −22.69 4.08 −9.47 −2.04 14.99
    下载: 导出CSV

    表  4  以混合茶为代表基质时6类茶叶中15种农药检测过程中产生的基质效应比较

    Table  4.   Matrix effects generated in detecting 15 pesticides in 6 types of tea with mixed tea used as a representative matrix

    农药名称
    Pesticide name
    基质效应 ME/%
    绿茶
    Green tea
    红茶
    Black tea
    花茶
    Scented tea
    黑茶
    Dark tea
    白茶
    White tea
    乌龙茶
    Oolong
    绝对平均值
    Absolute mean
    敌敌畏 Dichlorvos −26.54 −4.62 −21.14 −7.91 −2.00 0.13 10.39
    甲拌磷 Phorate −31.54 −7.56 −20.18 11.15 0.73 3.33 12.41
    五氯硝基苯 Pentachloronitrobenzene −4.26 −19.86 −5.49 −9.07 −3.37 4.01 7.68
    毒死蜱 Chlorpyrifos −6.62 −12.19 −7.30 −20.63 −1.45 4.01 8.70
    马拉硫磷 Malathion −18.27 0.98 −9.00 3.60 6.37 3.16 6.90
    杀螟硫磷 Fenitrothion −13.33 −4.13 −7.92 0.09 −4.73 4.24 5.74
    甲基异柳磷 Isofenphos-methy −1.50 −14.45 −5.17 −4.24 −2.66 0.54 4.76
    水胺硫磷 Isocarbophos −28.59 −17.63 −26.18 −13.29 −11.26 −4.39 16.89
    腐霉利 Procymidone −1.23 −15.46 −4.09 8.62 −2.73 1.39 5.59
    杀扑磷 Methidathion −48.09 27.31 −27.95 9.78 8.33 −7.07 21.42
    联苯菊酯 Bifenthrin −6.75 −12.74 −6.03 0.42 −0.73 0.66 4.55
    甲氰菊酯 Fenpropathrin −5.92 −6.60 −3.48 4.08 3.88 0.15 4.02
    氯菊酯 Permethrin −13.88 −16.75 −14.96 −2.25 −5.82 −3.65 9.55
    溴氰菊酯 Deltamethrin −22.58 −16.43 −15.17 3.73 −4.66 −2.17 10.79
    苯醚甲环唑 Difenoconazole −29.29 11.68 −13.66 16.24 1.11 9.40 13.56
    下载: 导出CSV

    表  5  添加水平为0.10 mg·kg−1时4种农药在两种定量方式下的平均回收率(n=6)

    Table  5.   Average recovery rates of 4 pesticides under two quantitative methods at an addition level of 0.10 mg·kg−1n=6)

    茶叶种类
    Tea types
    标液类型
    Standard liquid type
    马拉硫磷
    Malathion
    水胺硫磷
    Isocarbophos
    溴氰菊酯
    Deltamethrin
    苯醚甲环唑
    Difenoconazole
    平均回收率
    Average
    recovery
    rate/%
    相对标准
    偏差
    RSD/%
    平均回收率
    Average
    recovery
    rate/%
    相对标准
    偏差
    RSD/%
    平均回收率
    Average
    recovery
    rate/%
    相对标准
    偏差
    RSD/%
    平均回收率
    Average
    recovery
    rate/%
    相对标准
    偏差
    RSD/%
    绿茶
    Green tea
    绿茶基质标
    Green tea substrate
    114.993.18114.842.14112.752.16109.712.14
    混合茶基质标
    Mixed tea substrate
    107.764.1196.412.4693.091.63105.143.93
    花茶
    Scented tea
    花茶基质标
    Scented tea substrate
    90.473.46101.031.5785.544.9589.72.46
    混合茶基质标
    Mixed tea substrate
    91.92.5194.551.8390.553.1089.772.68
    红茶
    Black tea
    红茶基质标
    Black tea substrate
    76.573.10104.144.7187.783.3379.194.31
    混合茶基质标
    Mixed tea substrate
    85.244.84102.042.9791.254.8385.295.61
    黑茶
    Dark tea
    黑茶基质标
    Dark tea substrate
    84.032.56106.343.7980.542.9696.531.83
    混合茶基质标
    Mixed tea substrate
    94.832.85101.442.1187.112.4999.483.11
    白茶
    White tea
    白茶基质标
    White tea substrate
    78.883.6298.743.82107.185.1085.814.34
    混合茶基质标
    Mixed tea substrate
    80.585.12104.624.15105.032.6188.652.77
    乌龙茶
    Oolong
    乌龙茶基质标
    Oolong substrate
    86.463.94107.93.2180.182.2775.813.27
    混合茶基质标
    Mixed tea substrate
    88.63.81108.474.1983.233.1586.412.68
    下载: 导出CSV
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  • 收稿日期:  2023-12-19
  • 修回日期:  2024-04-19
  • 网络出版日期:  2024-07-10

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