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QuEChERS-气相色谱-串联质谱法测定中药材水蛭中73种农药残留

郑坤明

郑坤明. QuEChERS-气相色谱-串联质谱法测定中药材水蛭中73种农药残留[J]. 农药学学报, 2022, 24(3): 601-609. doi: 10.16801/j.issn.1008-7303.2021.0182
引用本文: 郑坤明. QuEChERS-气相色谱-串联质谱法测定中药材水蛭中73种农药残留[J]. 农药学学报, 2022, 24(3): 601-609. doi: 10.16801/j.issn.1008-7303.2021.0182
ZHENG Kunming. Determination of 73 pesticides in traditional Chinese medicine Hirudo by QuEChERS-gas chromatography-tandem mass spectrometry[J]. Chinese Journal of Pesticide Science, 2022, 24(3): 601-609. doi: 10.16801/j.issn.1008-7303.2021.0182
Citation: ZHENG Kunming. Determination of 73 pesticides in traditional Chinese medicine Hirudo by QuEChERS-gas chromatography-tandem mass spectrometry[J]. Chinese Journal of Pesticide Science, 2022, 24(3): 601-609. doi: 10.16801/j.issn.1008-7303.2021.0182

QuEChERS-气相色谱-串联质谱法测定中药材水蛭中73种农药残留

doi: 10.16801/j.issn.1008-7303.2021.0182
基金项目: 国家自然科学基金(21667007).
详细信息
    通讯作者:

    郑坤明,18198639783@163.com

  • 中图分类号: O657.263;TQ450.2

Determination of 73 pesticides in traditional Chinese medicine Hirudo by QuEChERS-gas chromatography-tandem mass spectrometry

Funds: Natural Science Foundation of China(21667007).
  • 摘要: 建立了中药材水蛭中73种农药的QuEChERS-气相色谱-串联质谱(GC-MS/MS)检测方法。样品用水浸泡并经V(乙酸) : V(乙腈) = 1 : 99和1.5 g乙酸钠溶液作为缓冲体系提取,采用优化的净化剂150 mg乙二胺-N-丙基甲硅烷(PSA)和150 mg十八烷基键合硅胶(C18)组合净化,经HP-5 MS色谱柱分离,在动态多反应监测模式下测定。结果表明:在优化的条件下,10.0~500 μg/L范围内,73种农药在水蛭中的峰面积与其质量浓度间呈良好的线性关系(r > 0.99)。在0.02、0.04和0.2 mg/kg 3个添加水平下,73种农药在水蛭中的回收率为71%~117%,相对标准偏差(RSD)(n = 6)为1.1%~12% (n = 6),定量限(LOQ)为0.02 mg/kg,检出限为0.001~0.008 mg/kg。本方法简捷、灵敏、稳定,可以满足实际检测需求。
  • 图  1  73种农药的总离子流图 (0.05 mg/L)

    Figure  1.  Total ion chromatogram of 73 pesticides (0.05 mg/L)

    图  2  不同吸附剂组成对提取回收率(70%~110%)的影响

    Figure  2.  Recoveries (70%-110%) of pesticides using different amounts of sorbents in the purification process

    图  3  3种复溶溶剂对水蛭空白样品的全扫描总离子流色谱图

    a:丙酮和正己烷 (V/V, 1/1)(Acetone/N-hexane, V/V, 1/1);b:乙酸乙酯 (Ethyl acetate);c:丙酮 (Acetone)

    Figure  3.  The full scan total ion current chromatograms of the blank Hirudo sample in three different solvents

    表  1  73种农药质谱参数

    Table  1.   Mass spectrum acquisition parameters of 73 pesticides

    编号
    No.
    农药
    Pesticide
    保留时间Retention
    time/min
    离子对Ion pair,
    m/z
    碰撞能量Collision
    energy/eV
    编号
    No.
    农药
    Pesticide
    保留时间Retention
    time/min
    离子对Ion pair,
    m/z
    碰撞能量Collision
    energy/eV
    1 敌敌畏 dichlorvos 6.14 109>79*
    184.9>93
    5
    10
    40 多效唑 paclobutrazol 12.38 236>125.1*
    236>167
    10
    10
    2 甲胺磷 methamidophos 6.76 141>95*
    141>79
    5
    15
    41 腐霉利 procymidone 12.26 96>67.1*
    96>53.1
    10
    15
    3 乙酰甲胺磷 acephate 8.43 136>94*
    136>42
    10
    5
    42 己唑醇 hexaconazole 13.16 231>175*
    256>82.1
    10
    10
    4 异丙威 isoprocarb 8.63 121>77.1*
    136>121.1
    20
    10
    43 甲拌磷砜 phorate sulfone 12.09 153>97*
    124.9>96.9
    10
    5
    5 α-六六六 α-HCH 9.83 218.9>183*
    216.9>181
    5
    42
    44 甲拌磷亚砜 Phorate sulfoxide 12.07 96.9>64.9*
    199>142.9
    20
    10
    6 二嗪磷 diazinon 10.09 137.1>84*
    137.1>54
    10
    20
    45 三唑醇-1 triadimenol-1 12.20 168>70*
    128>65
    10
    25
    7 甲拌磷 phorate 9.60 260>75*
    230.9>128.9
    5
    25
    46 三唑醇-2 triadimenol-2 12.10 168>70*
    128>65
    10
    25
    8 灭线磷 ethoprophos 9.14 157.9>97*
    157.9>114
    15
    5
    47 水胺硫磷 isocarbophos 12.15 135.9>108*
    135.9>69
    15
    30
    9 五氯硝基苯
    pentachloronitrobenzene
    10.23 295>237*
    236.9>142.9
    20
    30
    48 4,4'-滴滴滴 p,p'-DDD 13.15 234.9>165.1*
    236.9>165.2
    20
    9
    10 氧乐果 omethoate 9.82 155.9>110*
    109.9>79
    5
    15
    49 2,4'-滴滴涕 o,p'-DDT 13.17 235>165.2*
    237>165.2
    20
    12
    11 莠去津 atrazine 10.26 214.9>58.1*
    214.9>200.2
    10
    5
    50 4,4'-滴滴涕 p,p'-DDT 13.30 235>165.2*
    237>165.2
    20
    40
    12 治螟磷 sulfotep 9.48 201.8>145.9*
    237.8>145.9
    10
    10
    51 狄氏剂 dieldrin 12.75 262.9>193*
    277>241
    35
    5
    13 β-六六六 β-HCH 10.78 181>145*
    216.9>181
    15
    25
    52 联苯菊酯 bifenthrin 13.45 181.2>165.2*
    181.2>166.2
    25
    10
    14 γ-六六六 γ-HCH 10.88 181>145*
    216.9>181
    15
    10
    53 硫环磷 phosfolan 13.21 196>140*
    168>140
    10
    5
    15 久效磷 monocrotophos 10.38 127.1>109*
    127.1>95
    10
    15
    54 杀扑磷 methidathion 12.84 144.9>85*
    144.9>58.1
    5
    15
    16 抗蚜威 pirimicarb 11.09 238>166.2*
    166>55.1
    10
    20
    55 倍硫磷砜 fenthion sulfone 13.66 309.9>105*
    135.9>92
    10
    10
    17 乐果 dimethoate 10.76 86.9>46*
    142.9>111
    15
    10
    56 倍硫磷亚砜 fenthion sulfoxide 13.64 278>109*
    278>169
    15
    15
    18 氯唑磷 isazofos 10.75 161>119.1*
    161>146
    5
    5
    57 敌瘟磷 edifenphos 13.66 172.9>109*
    201>109
    5
    10
    19 西玛津 simazine 10.38 201.1>173.1*
    201.1>186.2
    5
    5
    58 高效氯氟氰菊酯-1
    lambda-cyhalothrin-1
    13.89 197>141*
    197>161
    10
    17
    20 乙草胺 acetochlor 10.89 222.9>132.2*
    222.9>147.2
    20
    5
    59 高效氯氟氰菊酯-2
    lambda-cyhalothrin-2
    13.99 197>141*
    197>161
    10
    46
    21 乙烯菌核利 vinclozolin 10.89 187>124*
    197.9>145
    20
    15
    60 甲氰菊酯 fenpropathrin 12.89 207.9>181*
    264.9>210
    5
    10
    22 δ-六六六 δ-HCH 11.20 217>181.1*
    181.1>145.1
    5
    25
    61 三唑磷 triazophos 13.74 161.2>134.2*
    161.2>106.1
    5
    10
    23 艾氏剂 aldrin 11.30 262.9>192.9*
    254.9>220
    35
    20
    62 乙螨唑 etoxazole 13.80 141>113*
    141>63.1
    15
    30
    24 毒死蜱 chlorpyrifos 11.59 196.9>169*
    198.9>171
    15
    15
    63 异菌脲 iprodione 13.87 187>124*
    243.9>187
    25
    5
    25 对硫磷 parathion 11.74 290.9>109*
    138.9>109
    10
    5
    64 哒螨灵 pyridaben 15.09 147.2>117.1*
    147.2>132.2
    20
    10
    26 二甲戊灵 pendimethalin 11.92 251.8>162.2*
    251.8>161.1
    10
    15
    65 伏杀硫磷 phosalone 14.54 182>111*
    182>102.1
    15
    15
    27 甲基毒死蜱 chlorpyrifos methyl 11.21 285.9>92.9*
    287.9>92.9
    20
    20
    66 氟胺氰菊酯 fluvalinate 16.03 250>55*
    250>200
    20
    20
    28 甲基对硫磷 parathion methyl 11.43 262.9>109*
    232.9>109
    10
    10
    67 氟氯氰菊酯 cyfluthrin 15.26 226>206*
    198.9>170.1
    15
    6
    29 甲基嘧啶磷 pirimiphos methyl 11.38 290>125*
    232.9>151
    20
    5
    68 氟氰戊菊酯-1 flucythrinate-1 15.75 156.9>107.1*
    198.9>157
    15
    10
    30 甲基异柳磷 isofenphos methyl 11.95 199>121*
    241.1>199.1
    10
    10
    69 氟氰戊菊酯-2 flucythrinate-2 15.77 156.9>107.1*
    198.9>157
    15
    10
    31 马拉硫磷 malathion 11.63 126.9>99*
    172.9>99
    5
    15
    70 腈苯唑 fenbuconazole 16.19 128.9>102.1*
    197.9>129
    15
    5
    32 三氯杀螨醇 dicofol 11.91 139>111*
    250.9>138.9
    15
    15
    71 氯菊酯 permethrin 14.94 183.1>168.1*
    183.1>153
    10
    24
    33 三唑酮 triadimefon 11.58 208>181.1*
    208>111
    5
    20
    72 氯氰菊酯 cypermethrin 15.26 163>91*
    163>127
    10
    15
    34 杀螟硫磷 fenitrothion 11.70 277>260*
    277>109
    5
    20
    73 亚胺硫磷 phosmet 14.65 160>77.1*
    160>133.1
    20
    10
    35 莠灭净 ametryn 11.42 227>58.1*
    227>170.1
    10
    10
    74 苯醚甲环唑 difenoconazole 18.18 322.8>264.8*
    264.9>202
    15
    20
    36 4,4'-滴滴伊 p,p'-DDE 12.62 246.1>176.2*
    315.8>246
    30
    9
    75 氰戊菊酯-1 fenvalerate-1 16.64 167>125.1*
    224.9>119
    5
    21
    37 倍硫磷 fenthion 11.96 278>109*
    278>169
    15
    15
    76 氰戊菊酯-2 fenvalerate-2 16.88 167>125.1*
    224.9>119
    5
    15
    38 丙溴磷 profenofos 12.72 207.9>63*
    338.8>268.7
    30
    15
    77 溴氰菊酯 deltamethrin 17.92 252.9>93*
    250.7>172
    15
    5
    39 丁草胺 butachlor 12.09 188.1>160.2*
    236.9>160.2
    10
    5
    注:*:定量离子对;表中−1、−2 表示目标物的同分异构体。Note: *: Quantitative ion pair; −1, −2 means isomers of compounds.
    下载: 导出CSV

    表  2  73种农药在水蛭中的检出限、平均回收率及相对标准偏差

    Table  2.   LOD, average recoveries and relative standard deviations(RSD) of 73 pesticides in Hirudo

    编号
    No.
    农药
    Pesticide
    添加水平 Spiked level检出限
    LOD/(mg/kg)
    基质效应
    Me/%
    0.02 mg/kg0.04 mg/kg0.2 mg/kg
    回收率
    Recovery/%
    RSD/%回收率
    Recovery/%
    RSD/%回收率
    Recovery/%
    RSD/%
    1 敌敌畏 dichlorvos 78 6.8 77 2.3 71 2.8 0.004 10.2
    2 甲胺磷 methamidophos 88 5.9 95 2.7 83 2.0 0.003 16.3
    3 乙酰甲胺磷 acephate 99 6.0 102 1.7 84 1.9 0.001 31.9
    4 异丙威 isoprocarb 85 9.6 99 3.5 85 6.0 0.003 11.4
    5 α-六六六 α-HCH 84 10 105 2.8 88 1.9 0.001 5.1
    6 二嗪磷 diazinon 76 5.4 78 5.3 89 2.4 0.001 12.0
    7 甲拌磷 phorate 88 9.2 104 3.2 89 2.1 0.001 17.1
    8 灭线磷 ethoprophos 109 6.0 111 2.5 91 1.8 0.001 7.6
    9 五氯硝基苯 pentachloronitrobenzene 86 5.0 91 1.9 95 2.1 0.002 −8.5
    10 氧乐果 omethoate 83 5.1 97 2.1 94 2.7 0.001 20.3
    11 莠去津 atrazine 91 4.3 96 2.7 93 1.6 0.002 3.1
    12 治螟磷 sulfotep 91 3.3 96 2.6 95 1.7 0.003 5.7
    13 β-六六六 β-HCH 89 3.5 98 2.4 97 1.7 0.002 4.8
    14 γ-六六六 γ-HCH 90 6.1 93 4.3 95 2.7 0.002 4.5
    15 久效磷 monocrotophos 100 6.5 101 3.4 105 4.0 0.003 14.0
    16 抗蚜威 pirimicarb 92 5.2 101 2.7 95 2.5 0.001 6.4
    17 乐果 dimethoate 93 5.9 93 3.8 93 2.3 0.002 12.3
    18 氯唑磷 isazofos 96 6.5 104 3.5 95 2.0 0.005 10.5
    19 西玛津 simazine 90 5.2 101 3.7 97 2.4 0.008 11.1
    20 乙草胺 acetochlor 96 4.8 101 3.6 104 2.2 0.001 5.0
    21 乙烯菌核利 vinclozolin 98 6.3 101 3.2 101 2.2 0.002 4.6
    22 δ-六六六 δ-HCH 96 5.4 100 3.8 101 2.0 0.007 3.1
    23 艾氏剂 aldrin 97 5.5 101 3.4 103 2.5 0.004 −0.5
    24 毒死蜱 chlorpyrifos 97 6.6 104 3.1 101 1.8 0.005 0.7
    25 对硫磷 parathion 87 5.4 104 3.3 103 1.9 0.003 22.8
    26 二甲戊灵 pendimethalin 87 7.0 105 3.3 101 3.0 0.002 19.0
    27 甲基毒死蜱 chlorpyrifos methyl 96 5.5 105 2.8 101 1.7 0.002 2.0
    28 甲基对硫磷 parathion methyl 101 5.8 106 3.7 106 2.0 0.004 12.1
    29 甲基嘧啶磷 pirimiphos methyl 91 8.1 95 5.1 105 1.3 0.001 4.5
    30 甲基异柳磷 isofenphos methyl 89 3.6 102 3.1 102 1.3 0.003 5.1
    31 马拉硫磷 malathion 96 4.2 108 4.0 107 2.8 0.007 16.0
    32 三氯杀螨醇 dicofol 79 5.8 109 4.0 110 2.4 0.004 −2.5
    33 三唑酮 triadimefon 98 7.9 98 4.5 112 1.3 0.003 4.6
    34 杀螟硫磷 fenitrothion 98 5.6 103 4.1 107 2.4 0.004 25.7
    35 莠灭净 ametryn 100 5.8 105 2.7 89 2.7 0.003 −1.4
    36 4,4′-滴滴伊 p,p′-DDE 101 5.0 100 2.4 91 3.4 0.002 2.5
    37 倍硫磷 fenthion 91 4.9 97 2.6 88 3.4 0.002 −27.6
    38 丙溴磷 profenofos 102 5.8 103 2.6 93 3.0 0.003 16.1
    39 丁草胺 butachlor 96 5.4 100 2.5 91 3.1 0.006 16.6
    40 多效唑 paclobutrazol 96 5.6 102 3.4 92 3.3 0.001 16.1
    41 腐霉利 procymidone 101 5.2 105 2.5 93 2.9 0.005 0.2
    42 己唑醇 hexaconazole 96 6.7 103 4.0 90 3.2 0.005 −3.9
    43 甲拌磷砜 phoratesulfone 96 5.9 102 2.9 91 2.7 0.008 16.0
    44 甲拌磷亚砜 phoratesulfoxide 98 8.9 110 4.6 96 4.8 0.007 14.5
    45 三唑醇-1 triadimenol-1 99 9.8 117 4.1 97 5.0 0.004 15.8
    46 三唑醇-2 triadimenol-2 102 7.4 106 4.3 92 3.9 0.007 11.2
    47 水胺硫磷 isocarbophos 101 5.0 104 3.2 92 2.5 0.008 22.4
    48 4,4′-滴滴滴 p,p′-DDD 109 8.9 113 4.6 99 3.5 0.001 19.2
    49 2,4′-滴滴涕 o,p′-DDT 104 8.0 107 4.1 89 3.7 0.002 1.8
    50 4,4′-滴滴涕 p,p′-DDT 105 7.9 109 3.8 90 2.9 0.002 18.3
    51 狄氏剂 dieldrin 107 9.6 110 6.1 91 4.1 0.002 −4.2
    52 联苯菊酯 bifenthrin 108 8.0 109 4.8 91 3.7 0.002 14.7
    53 硫环磷 phosfolan 100 8.6 113 5.5 94 3.5 0.002 38.4
    54 杀扑磷 methidathion 113 7.5 114 4.4 94 5.2 0.005 16.3
    55 倍硫磷砜 fenthion sulfone 99 9.3 114 5.0 94 5.1 0.001 −31.7
    56 倍硫磷亚砜 fenthion sulfoxide 111 9.4 97 5.9 93 5.8 0.003 −39.8
    57 敌瘟磷 edifenphos 99 9.5 105 6.4 89 6.9 0.003 19.3
    58 高效氯氟氰菊酯-1 lambda-cyhalothrin-1 98 9.9 96 6.5 89 6.2 0.002 30.9
    59 高效氯氟氰菊酯-2 lambda-cyhalothrin-2 92 8.1 100 5.5 88 7.6 0.002 28.4
    60 甲氰菊酯 fenpropathrin 91 12 96 7.5 91 2.1 0.004 11.2
    61 三唑磷 triazophos 92 9.8 98 6.8 87 3.9 0.007 17.1
    62 乙螨唑 etoxazole 93 8.2 97 7.2 89 7.2 0.006 14.2
    63 异菌脲 iprodione 98 2.6 99 9.2 90 3.6 0.006 17.3
    64 哒螨灵 pyridaben 102 3.8 102 11 90 3.7 0.002 30.8
    65 伏杀硫磷 phosalone 94 3.4 94 4.8 89 3.3 0.004 28.2
    66 氟胺氰菊酯 fluvalinate 95 9.5 100 8.3 91 3.0 0.006 48.7
    67 氟氯氰菊酯 cyfluthrin 94 2.0 107 9.3 90 2.8 0.006 18.1
    68 氟氰戊菊酯-1 flucythrinate-1 96 2.7 98 10 91 3.7 0.001 31.8
    69 氟氰戊菊酯-2 flucythrinate-2 99 1.4 93 1.9 88 1.1 0.002 32.2
    70 腈苯唑 fenbuconazole 103 2.7 98 2.1 93 1.7 0.003 30.0
    71 氯菊酯 permethrin 101 2.5 100 2.7 91 2.3 0.008 18.1
    72 氯氰菊酯 cypermethrin 96 5.6 99 2.6 89 2.5 0.002 18.1
    73 亚胺硫磷 phosmet 102 2.7 109 2.4 93 1.1 0.007 30.2
    74 苯醚甲环唑 difenoconazole 93 3.7 103 4.3 89 1.2 0.006 51.6
    75 氰戊菊酯-1 fenvalerate-1 95 2.7 102 3.4 91 2.1 0.002 99.0
    76 氰戊菊酯-2 fenvalerate-2 115 2.2 114 2.7 95 2.7 0.007 102.9
    77 溴氰菊酯 deltamethrin 98 3.2 109 3.8 92 1.6 0.002 15.2
    注:表中−1、−2 表示化合物的同分异构体。Note: −1,−2 means isomers of compounds.
    下载: 导出CSV
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  • 收稿日期:  2021-08-30
  • 录用日期:  2022-01-05
  • 网络出版日期:  2022-04-07
  • 刊出日期:  2022-06-10

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