Optimization of a Multiresidue Analysis of 65 Pesticides in Surface Water Using Solid-Phase Extraction by LC-MS/MS
Abstract
:1. Introduction
2. Results and Discussion
2.1. Optimization of LC-MS/MS Conditions
2.2. Optimization of the SPE Method
2.2.1. Sorbent Type
2.2.2. Eluent
2.2.3. Sorbent Drying Time
2.2.4. Pretreatment
2.3. Application to Real Samples
3. Materials and Methods
3.1. Chemicals and Reagents
3.2. Standards
3.3. Samples
3.4. Sample Preparation
3.5. Liquid Chromatography-Tandem Mass Spectrometry
3.5.1. Liquid Chromatography Separation Conditions
3.5.2. Mass Spectroscopy Conditions
3.6. Method Validation
3.6.1. Instrumental Linearity
3.6.2. Method Detection and Reporting Limit
3.6.3. Accuracy and Precision
4. Conclusions
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Acknowledgments
Conflicts of Interest
Sample Availability
References
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Compound | RT (min) | Precursor Ion | Quantification Transition (m/z) | DP (eV) | CE (eV) | Confirmatory Transition (m/z) | DP (eV) | CE (eV) |
---|---|---|---|---|---|---|---|---|
Positive Mode | ||||||||
Acetamiprid | 3.19 | 223.0 | 125.9 | 56 | 25 | 89.9 | 56 | 43 |
Atazine | 6.00 | 216.0 | 174.0 | 61 | 25 | 103.9 | 61 | 37 |
Azoxystrobin | 7.10 | 404.0 | 371.9 | 41 | 19 | 344.0 | 41 | 33 |
Bensulide | 8.57 | 397.9 | 313.8 | 31 | 15 | 157.9 | 31 | 31 |
Boscalid | 7.38 | 342.9 | 306.9 | 101 | 25 | 270.9 | 101 | 43 |
Bromacil | 4.88 | 260.9 | 204.9 | 26 | 17 | 187.8 | 26 | 37 |
Carbaryl | 5.35 | 202.0 | 145.0 | 31 | 13 | 127.0 | 31 | 37 |
Chlorantraniliprole | 6.70 | 483.9 | 285.8 | 51 | 17 | 452.9 | 51 | 21 |
Chlorsulfuron | 5.32 | 357.9 | 141.0 | 106 | 21 | 167.1 | 106 | 21 |
Chlorpyrifos | 10.46 | 349.8 | 197.9 | 41 | 25 | 96.8 | 41 | 45 |
Chlothianidin | 2.86 | 249.9 | 168.9 | 36 | 15 | 131.9 | 36 | 19 |
Cyprodinil | 8.28 | 226.0 | 93.0 | 81 | 41 | 108.1 | 81 | 35 |
Cyantraniliprole | 5.68 | 473.0 | 284.0 | 76 | 17 | 442.0 | 76 | 29 |
Diazinon | 8.89 | 305.0 | 169.0 | 66 | 29 | 153.0 | 66 | 27 |
Dichlorvos | 4.87 | 220.9 | 108.9 | 86 | 23 | 78.9 | 86 | 34 |
3,4-dichloroaniline | 7.00 | 161.9 | 127.0 | 140 | 30 | 109.0 | 140 | 40 |
Diflubenzuron | 8.37 | 310.7 | 157.9 | 41 | 17 | 140.8 | 41 | 41 |
Dimethoate | 3.14 | 229.9 | 198.9 | 21 | 13 | 124.8 | 21 | 27 |
Dinotefuran | 2.03 | 203.0 | 129.1 | 43 | 14 | 114.0 | 43 | 16 |
Dithiopyr | 9.79 | 402.0 | 354.0 | 116 | 23 | 272.0 | 116 | 37 |
Diuron | 6.22 | 232.9 | 72.0 | 46 | 21 | 46.1 | 46 | 35 |
Ethoprophos | 8.10 | 242.9 | 173.0 | 61 | 19 | 130.7 | 61 | 27 |
Fenamidone | 7.30 | 311.9 | 236.0 | 56 | 19 | 92.0 | 56 | 39 |
Fenhexamid | 8.03 | 301.9 | 97.1 | 21 | 29 | 54.9 | 21 | 59 |
Fludioxonil | 7.33 | 265.9 | 229.0 | 20 | 13 | 158.0 | 20 | 43 |
Flupyradifurone | 3.22 | 289.0 | 126.1 | 105 | 27 | 90.0 | 105 | 58 |
Hexazinone | 4.94 | 253.1 | 171.0 | 41 | 21 | 71.0 | 41 | 39 |
Imidacloprid | 2.80 | 256.0 | 208.9 | 30 | 21 | 175.1 | 30 | 25 |
Indoxacarb | 9.70 | 527.8 | 150.1 | 76 | 27 | 202.9 | 76 | 49 |
Isoxaben | 7.55 | 333.1 | 165.0 | 41 | 23 | 107.0 | 41 | 79 |
Kresoxim-Methyl | 8.63 | 331.1 | 314.0 | 24 | 7 | 206.0 | 24 | 13 |
Linuron | 6.96 | 249.0 | 182.0 | 51 | 23 | 160.0 | 51 | 25 |
Malathion | 7.49 | 330.9 | 126.9 | 31 | 17 | 284.9 | 31 | 11 |
Mefenoxam | 6.29 | 280.0 | 220.0 | 21 | 19 | 248.0 | 21 | 13 |
Methidathion | 6.39 | 319.8 | 302.9 | 6 | 9 | 144.9 | 6 | 17 |
Methomyl | 2.05 | 163.0 | 87.8 | 11 | 13 | 105.9 | 11 | 13 |
Methoxyfenozide | 7.62 | 369.1 | 149.0 | 36 | 21 | 313.1 | 36 | 11 |
Metribuzin | 4.81 | 215.1 | 187.0 | 36 | 25 | 84.0 | 36 | 31 |
Norflurazon | 6.39 | 303.9 | 284.0 | 101 | 31 | 159.9 | 101 | 39 |
Oryzalin | 8.22 | 347.0 | 304.9 | 41 | 19 | 288.0 | 41 | 23 |
Oxadiazon | 10.31 | 344.9 | 302.9 | 91 | 17 | 219.9 | 91 | 27 |
Prometon | 5.96 | 226.1 | 142.0 | 56 | 31 | 184.1 | 56 | 25 |
Prometryn | 7.48 | 242.0 | 157.9 | 45 | 31 | 200 | 45 | 25 |
Propanil | 6.99 | 217.9 | 161.9 | 56 | 21 | 126.9 | 56 | 33 |
Propargite | 10.82 | 368.1 | 231.1 | 21 | 13 | 175.0 | 21 | 21 |
Propiconazole | 8.93 | 341.9 | 158.9 | 56 | 31 | 69.0 | 56 | 23 |
Pyraclostrobin | 9.08 | 388.0 | 193.9 | 36 | 17 | 163.0 | 36 | 31 |
Pyriproxyfen | 10.34 | 322.0 | 95.9 | 46 | 19 | 184.9 | 46 | 29 |
Quinoxyfen | 10.43 | 307.8 | 196.8 | 121 | 43 | 161.9 | 121 | 47 |
Simazine | 4.88 | 202.0 | 124.0 | 61 | 25 | 103.9 | 61 | 33 |
S-Metolachlor | 8.20 | 284.0 | 252.0 | 41 | 19 | 176.1 | 41 | 35 |
Sulfoxaflor | 3.42 | 278.1 | 154.1 | 66 | 13 | 154.1 | 66 | 38 |
Tebuconazole | 8.79 | 308.0 | 69.9 | 66 | 57 | 124.9 | 66 | 39 |
Tebufenozide | 8.49 | 353.1 | 133.0 | 26 | 23 | 297.1 | 26 | 11 |
Tebuthiuron | 5.05 | 229.0 | 172.0 | 46 | 23 | 115.8 | 46 | 35 |
Thiacloprid | 3.59 | 252.9 | 125.8 | 76 | 27 | 90.0 | 76 | 51 |
Thiamethoxam | 2.15 | 291.9 | 211.0 | 41 | 19 | 180.9 | 41 | 29 |
Thiobencarb | 9.25 | 258.0 | 124.9 | 41 | 23 | 89.0 | 41 | 65 |
Trifloxystrobin | 9.69 | 409.0 | 186.0 | 41 | 23 | 144.9 | 41 | 57 |
Atrazine-d5 (Surrogate) | 5.94 | 220.9 | 179.0 | 61 | 25 | 101.0 | 61 | 31 |
Imidacloprid-d4 (Surrogate) | 2.77 | 259.9 | 213.0 | 170 | 46 | 179.0 | 170 | 46 |
Negative Mode | ||||||||
Fipronil | 8.55 | 436.8 | 329.8 | −45 | −22 | 331.8 | −45 | −22 |
Fipronil Amide | 6.62 | 452.7 | 347.9 | −25 | −20 | 303.9 | −25 | −32 |
Fipronil Sulfide | 8.75 | 418.8 | 382.8 | −20 | −18 | 261.5 | −20 | −38 |
Fipronil Sulfone | 9.01 | 450.8 | 414.9 | −40 | −22 | 281.8 | −40 | −36 |
Desulfinyl Fipronil | 8.35 | 387.0 | 350.9 | −45 | −16 | 281.8 | −45 | −42 |
Desulfinyl Fipronil Amide | 5.61 | 405.0 | 369.0 | −50 | −12 | 329.0 | −50 | −30 |
Analyte (ng/mL) | SW1 | SW2 | SW3 | SW4 | SW5 | SW6 | SW7 | SW8 | SW9 | SW10 |
---|---|---|---|---|---|---|---|---|---|---|
Acetamiprid | ND | ND | ND | ND | ND | ND | Trace | 0.0977 | 0.123 | Trace |
Atrazine | ND | ND | ND | ND | ND | ND | ND | ND | ND | ND |
Azoxystrobin | Trace | Trace | ND | Trace | Trace | Trace | 0.158 | 0.0338 | Trace | Trace |
Bensulide | ND | ND | ND | Trace | ND | ND | 0.9710 | 7.53 | 52.3 | 0.083 |
Boscalid | ND | ND | ND | Trace | ND | ND | 0.852 | 1.27 | 0.565 | Trace |
Bromacil | Trace | ND | ND | Trace | ND | ND | ND | ND | ND | ND |
Carbaryl | ND | Trace | ND | Trace | ND | ND | ND | ND | ND | ND |
Chlorantraniliprole | Trace | ND | ND | Trace | Trace | 0.0205 | 0.062 | 0.229 | 0.515 | Trace |
Chlorsulfuron | ND | ND | ND | ND | ND | ND | ND | ND | ND | ND |
Chlorpyrifos | ND | ND | ND | ND | ND | ND | ND | ND | ND | ND |
Clothianidin | Trace | 0.0228 | 0.0318 | Trace | Trace | Trace | 0.0956 | 0.90 | 0.550 | Trace |
Cyprodinil | ND | ND | ND | ND | ND | ND | Trace | ND | 0.103 | ND |
Cyantraniliprole | ND | ND | ND | ND | ND | ND | 0.111 | 0.517 | 0.164 | 0.0568 |
Diazinon | ND | ND | ND | ND | ND | ND | ND | ND | ND | ND |
Dichlorvos | ND | ND | ND | ND | ND | ND | ND | ND | ND | ND |
3,4-dicloroaniline | ND | ND | ND | ND | ND | ND | ND | ND | ND | ND |
Diflubenzuron | ND | ND | ND | ND | ND | ND | ND | ND | ND | ND |
Dimethoate | ND | ND | ND | ND | ND | ND | ND | ND | ND | ND |
Dinotefuran | 0.0478 | 0.0262 | 0.0212 | 0.041 | 0.0371 | Trace | ND | ND | ND | ND |
Dithiopyr | Trace | 0.0227 | 0.0252 | Trace | Trace | 0.0326 | ND | ND | ND | ND |
Diuron | 0.0264 | 0.128 | 0.0721 | Trace | Trace | 0.0252 | ND | ND | ND | ND |
Ethoprop | ND | ND | ND | ND | ND | ND | ND | ND | ND | ND |
Fenamidone | ND | ND | ND | ND | ND | ND | Trace | Trace | Trace | ND |
Fenhexamid | ND | ND | ND | ND | ND | ND | ND | ND | ND | ND |
Fludioxonil | ND | ND | ND | ND | ND | ND | 0.0143 | ND | 0.0664 | ND |
Flupyradifurone | ND | ND | ND | ND | ND | ND | 0.0865 | 0.115 | 0.274 | ND |
Hexazinone | ND | ND | ND | ND | ND | ND | ND | ND | ND | ND |
Imidacloprid | 0.0397 | 0.0463 | 0.0274 | 0.263 | 0.0300 | 0.0256 | 0.148 | 0.254 | 0.159 | ND |
Indoxacarb | ND | ND | ND | ND | ND | ND | ND | ND | ND | ND |
Isoxaben | ND | ND | ND | ND | ND | Trace | ND | ND | ND | ND |
Kresoxim-Methyl | Trace | Trace | Trace | Trace | Trace | ND | ND | 0.0292 | 0.296 | ND |
Linuron | ND | ND | ND | ND | ND | ND | ND | ND | ND | ND |
Malathion | ND | ND | ND | ND | ND | ND | ND | ND | ND | ND |
Mefenoxam | ND | ND | ND | ND | ND | ND | 0.0299 | 0.0245 | 0.0207 | ND |
Methidathion | ND | ND | ND | Trace | Trace | ND | ND | ND | ND | ND |
Methomyl | ND | ND | ND | ND | ND | ND | 0.30 | 0.399 | 3.43 | 0.0224 |
Methoxyfenozide | ND | ND | ND | Trace | ND | ND | Trace | 0.0312 | 0.0333 | ND |
Metribuzin | ND | ND | ND | 0.0292 | ND | ND | ND | ND | ND | ND |
Norflurazon | ND | ND | ND | ND | ND | ND | ND | ND | ND | ND |
Oryzalin | Trace | Trace | ND | Trace | ND | ND | ND | ND | ND | ND |
Oxadiazon | Trace | ND | ND | ND | Trace | Trace | ND | ND | ND | ND |
Prometon | ND | ND | ND | ND | ND | ND | ND | ND | ND | ND |
Prometryn | ND | ND | ND | ND | ND | ND | 0.159 | Trace | Trace | 0.0493 |
Propanil | ND | ND | ND | ND | ND | ND | ND | ND | ND | ND |
Propargite | ND | ND | ND | ND | ND | ND | ND | ND | ND | ND |
Propiconazole | Trace | Trace | Trace | Trace | 0.0278 | Trace | 0.0236 | ND | Trace | ND |
Pyraclostrobin | ND | ND | ND | ND | ND | ND | 0.135 | Trace | 0.021 | ND |
Pyriproxyfen | ND | ND | ND | ND | ND | ND | ND | ND | ND | ND |
Quinoxyfen | ND | ND | ND | ND | ND | ND | Trace | ND | Trace | ND |
Simazine | ND | ND | ND | ND | ND | ND | Trace | ND | ND | ND |
S-Metolachlor | ND | ND | ND | ND | ND | ND | ND | Trace | ND | ND |
Sulfoxaflor | ND | ND | ND | ND | ND | ND | 0.025 | 0.684 | 0.566 | ND |
Tebuconazole | 0.0501 | 0.0719 | Trace | 0.0772 | Trace | Trace | ND | ND | ND | ND |
Tebufenozide | ND | ND | ND | ND | ND | ND | ND | ND | ND | ND |
Tebuthiuron | ND | ND | ND | Trace | ND | ND | ND | ND | ND | ND |
Thiacloprid | ND | ND | ND | ND | ND | ND | ND | ND | ND | ND |
Thiamethoxam | Trace | 0.0591 | Trace | 0.0207 | 0.0296 | 0.0575 | 0.0701 | 0.371 | 1.13 | 0.0221 |
Thiobencarb | ND | ND | ND | ND | ND | ND | ND | ND | ND | ND |
Trifloxystrobin | ND | ND | ND | ND | ND | ND | ND | Trace | ND | ND |
Atrazine-d5 (Surrogate) | 0.0407 | 0.0406 | 0.0426 | 0.0405 | 0.0407 | 0.0412 | 0.05 | 0.0468 | 0.0425 | 0.0426 |
Imidacloprid-d4 (Surrogate) | 0.0459 | 0.0412 | 0.0418 | 0.0376 | 0.0426 | 0.0415 | 0.054 | 0.0526 | 0.0363 | 0.0437 |
Fipronil | 0.0273 | 0.0290 | Trace | 0.141 | 0.0803 | 0.0249 | ND | ND | ND | ND |
Fipronil Amide | Trace | Trace | Trace | 0.022 | Trace | Trace | ND | ND | ND | ND |
Fipronil Sulfide | Trace | Trace | Trace | Trace | Trace | Trace | ND | ND | ND | ND |
Fipronil Sulfone | 0.0383 | 0.0345 | 0.0836 | 0.110 | 0.0846 | 0.0398 | ND | ND | ND | ND |
Desulfinyl Fipronil | Trace | 0.0238 | Trace | 0.0957 | 0.074 | 0.0214 | ND | ND | ND | ND |
Desulfinyl Fipronil Amide | Trace | Trace | Trace | Trace | Trace | Trace | ND | ND | ND | ND |
Compound | SD (ng/mL) | RL (ng/mL) | Compound | SD (ng/mL) | RL (ng/mL) |
---|---|---|---|---|---|
Acetamiprid | 0.00038 | 0.00238 | Methidathion NH4 | 0.00026 | 0.00163 |
Atrazine | 0.00042 | 0.00261 | Methomyl | 0.00026 | 0.00163 |
Azoxystrobin | 0.00051 | 0.00318 | Methoxyfenozide | 0.00037 | 0.00231 |
Bensulide | 0.00021 | 0.00133 | Metribuzin | 0.00065 | 0.00410 |
Boscalid | 0.00055 | 0.00345 | Norflurazon | 0.00027 | 0.00169 |
Bromacil | 0.00037 | 0.00230 | Oryzalin | 0.00101 | 0.00637 |
Carbaryl | 0.00052 | 0.00329 | Oxadiazon | 0.00048 | 0.00300 |
Chlorantraniliprole | 0.00041 | 0.00257 | Prometon | 0.00032 | 0.00200 |
Chlorsulfuron | 0.00039 | 0.00246 | Prometryn | 0.00040 | 0.00253 |
Chlorpyrifos | 0.00041 | 0.00257 | Propanil | 0.00058 | 0.00366 |
Clothianidin | 0.00066 | 0.00417 | propargite NH4 | 0.00028 | 0.00174 |
Cyprodinil | 0.00027 | 0.00170 | Propiconazole | 0.00041 | 0.00255 |
Cyantraniliprole | 0.00068 | 0.00428 | Pyraclostrobin | 0.00031 | 0.00195 |
Diazinon | 0.00055 | 0.00344 | Pyriproxyfen | 0.00026 | 0.00164 |
Dichlorvos | 0.00038 | 0.00237 | Quinoxyfen | 0.00058 | 0.00366 |
3,4-dicloroaniline | 0.00046 | 0.00289 | Simazine | 0.00024 | 0.00149 |
Diflubenzuron | 0.00033 | 0.00208 | S-Metolachlor | 0.00041 | 0.00259 |
Dimethoate | 0.00042 | 0.00264 | Sulfoxaflor | 0.00067 | 0.00419 |
Dinotefuran | 0.00030 | 0.00187 | Tebuconazole | 0.00076 | 0.00475 |
Dithiopyr | 0.00029 | 0.00180 | Tebufenozide | 0.00032 | 0.00202 |
Diuron | 0.00020 | 0.00128 | Tebuthiuron | 0.00040 | 0.00250 |
Ethopropos | 0.00050 | 0.00316 | Thiacloprid | 0.00051 | 0.00321 |
Fenamidone | 0.00067 | 0.00420 | Thiamethoxam | 0.00054 | 0.00341 |
Fenhexamid | 0.00082 | 0.00517 | Thiobencarb | 0.00042 | 0.00265 |
Fludioxonil NH4 | 0.00068 | 0.00429 | Trifloxystrobin | 0.00029 | 0.00180 |
Flupyradifurone | 0.00036 | 0.00225 | Atrazine-d5 | 0.00043 | 0.00273 |
Hexazinone | 0.00045 | 0.00286 | Imidacloprid-d4 | 0.00095 | 0.00594 |
Imidacloprid | 0.00085 | 0.00537 | Fipronil | 0.00028 | 0.00175 |
Indoxacarb | 0.00106 | 0.00667 | Fipronil Amide | 0.00088 | 0.00551 |
Isoxaben | 0.00032 | 0.00201 | Fipronil Sulfide | 0.00066 | 0.00412 |
Kresoxim-Methyl NH4 | 0.00071 | 0.00446 | Fipronil Sulfone | 0.00025 | 0.00155 |
Linuron | 0.00039 | 0.00247 | Desulfinyl Fipronil | 0.00033 | 0.00208 |
Malathion | 0.00028 | 0.00177 | Desulfinyl Fipronil Amide | 0.00056 | 0.00352 |
Mefenoxam | 0.00027 | 0.00167 |
Analyte | Concentration (ng/mL) | Mean Recovery (%) | RSD (%) | Analyte | Concentration (ng/mL) | Mean Recovery (%) | RSD (%) | Analyte | Concentration (ng/mL) | Mean Recovery (%) | RSD (%) |
---|---|---|---|---|---|---|---|---|---|---|---|
Acetamipirid | 0.02 | 104.7 | 2.8 | Cyprodinil | 0.02 | 104.8 | 7.5 | Fenamidone | 0.02 | 101.1 | 4.5 |
0.05 | 109.2 | 3.8 | 0.05 | 106.9 | 4.4 | 0.05 | 105.6 | 6.6 | |||
0.1 | 105.6 | 7.6 | 0.1 | 105.1 | 7.3 | 0.1 | 106.9 | 3.9 | |||
Atrazine | 0.02 | 104.5 | 2.7 | Cyantraniliprole | 0.02 | 92.9 | 3.0 | Fenhexamid | 0.02 | 89.5 | 10.2 |
0.05 | 110.0 | 3.6 | 0.05 | 95.9 | 12.7 | 0.05 | 89.1 | 11.8 | |||
0.1 | 110.2 | 5.5 | 0.1 | 87.8 | 11.7 | 0.1 | 83.6 | 5.9 | |||
Azoxystrobin | 0.02 | 103.4 | 3.0 | Diazinon | 0.02 | 94.9 | 4.9 | Fludioxonil | 0.02 | 89.9 | 4.7 |
0.05 | 109.0 | 5.7 | 0.05 | 100.9 | 9.4 | 0.05 | 105.1 | 6.6 | |||
0.1 | 105.8 | 7.1 | 0.1 | 101.6 | 7.8 | 0.1 | 104.4 | 5.2 | |||
Bensulide | 0.02 | 96.1 | 5.6 | Dichlorvos | 0.02 | 81.1 | 7.2 | Flupyradifurone | 0.02 | 106.5 | 0.4 |
0.05 | 100.7 | 8.3 | 0.05 | 82.2 | 14.3 | 0.05 | 111.5 | 3.9 | |||
0.1 | 101.9 | 11.6 | 0.1 | 76.2 | 11.7 | 0.1 | 109.5 | 3.8 | |||
Boscalid | 0.02 | 108.8 | 2.5 | 3,4-dichloroaniline | 0.02 | 103.7 | 3.9 | Hexazinone | 0.02 | 98.5 | 8.5 |
0.05 | 110.1 | 6.8 | 0.05 | 106.1 | 7.1 | 0.05 | 101.5 | 8.5 | |||
0.1 | 109.4 | 6.3 | 0.1 | 106.2 | 3.7 | 0.1 | 102.2 | 4.2 | |||
Bromacil | 0.02 | 91.3 | 9.6 | Diflubenzuron | 0.02 | 94.1 | 3.3 | Imidacloprid | 0.02 | 100.4 | 3.6 |
0.05 | 94.6 | 9.6 | 0.05 | 95.5 | 11.3 | 0.05 | 105.2 | 5.4 | |||
0.1 | 88.8 | 5.9 | 0.1 | 88.5 | 6.7 | 0.1 | 102.0 | 7.8 | |||
Carbaryl | 0.02 | 96.3 | 7.5 | Dimethoate | 0.02 | 102.5 | 2.1 | Indoxacarb | 0.02 | 85.0 | 7.0 |
0.05 | 108.4 | 3.0 | 0.05 | 106.9 | 4.5 | 0.05 | 90.5 | 5.8 | |||
0.1 | 111.5 | 2.9 | 0.1 | 109.1 | 2.0 | 0.1 | 90.6 | 12.8 | |||
Chlorantraniliprole | 0.02 | 99.5 | 5.8 | Dinotefuran | 0.02 | 97.1 | 2.5 | Isoxaben | 0.02 | 106.4 | 3.1 |
0.05 | 98.2 | 10.8 | 0.05 | 101.6 | 5.2 | 0.05 | 111.3 | 2.8 | |||
0.1 | 93.1 | 10.6 | 0.1 | 70.4 | 8.8 | 0.1 | 108.9 | 5.1 | |||
Chlorsulfuron | 0.02 | 96.3 | 9.2 | Dithiopyr | 0.02 | 93.6 | 3.7 | Kresoxim-Methyl NH4 | 0.02 | 82.3 | 5.4 |
0.05 | 99.6 | 13.2 | 0.05 | 100.0 | 9.8 | 0.05 | 99.4 | 3.9 | |||
0.1 | 91.1 | 5.7 | 0.1 | 100.3 | 10.5 | 0.1 | 100.0 | 7.1 | |||
Chlorpyrifos | 0.02 | 78.1 | 6.9 | Diuron | 0.02 | 99.0 | 3.9 | Linuron | 0.02 | 105.1 | 1.7 |
0.05 | 79.6 | 8.7 | 0.05 | 107.6 | 6.0 | 0.05 | 109.4 | 5.2 | |||
0.1 | 77.5 | 8.5 | 0.1 | 108.5 | 4.6 | 0.1 | 107.5 | 5.4 | |||
Chlothianidin | 0.02 | 89.9 | 5.8 | Ethopropos | 0.02 | 105.2 | 4.9 | Malathion | 0.02 | 100.4 | 3.4 |
0.05 | 92.3 | 12.7 | 0.05 | 107.8 | 6.1 | 0.05 | 106.5 | 6.2 | |||
0.1 | 89.1 | 8.0 | 0.1 | 109.9 | 3.4 | 0.1 | 106.8 | 4.4 | |||
Mefenoxam | 0.02 | 106.9 | 2.4 | Propiconazole | 0.02 | 98.0 | 1.9 | Thiobencarb | 0.02 | 89.6 | 5.0 |
0.05 | 109.9 | 3.6 | 0.05 | 104.8 | 5.8 | 0.05 | 92.7 | 8.0 | |||
0.1 | 109.6 | 3.8 | 0.1 | 104.0 | 5.9 | 0.1 | 95.0 | 7.9 | |||
Methidathion NH4 | 0.02 | 99.3 | 0.7 | Pyraclostrobin | 0.02 | 100.4 | 5.2 | Trifloxystrobin | 0.02 | 98.9 | 3.8 |
0.05 | 108.3 | 5.4 | 0.05 | 102.6 | 7.8 | 0.05 | 101.5 | 4.6 | |||
0.1 | 107.8 | 5.4 | 0.1 | 101.2 | 8.6 | 0.1 | 99.4 | 7.3 | |||
Methomyl | 0.02 | 76.0 | 5.6 | Pyriproxyfen | 0.02 | 72.0 | 2.8 | Atrzaine-d5 | 0.02 | 103.2 | 5.4 |
0.05 | 81.2 | 7.0 | 0.05 | 72.0 | 5.1 | 0.05 | 109.3 | 4.3 | |||
0.1 | 73.2 | 11.6 | 0.1 | 70.5 | 6.6 | 0.1 | 107.9 | 5.2 | |||
Methoxyfenozide | 0.02 | 110.8 | 2.9 | Quinoxyfen | 0.02 | 72.6 | 3.6 | Imidacloprid-d4 | 0.02 | 98.9 | 12.6 |
0.05 | 113.3 | 1.8 | 0.05 | 73.5 | 6.2 | 0.05 | 102.3 | 9.5 | |||
0.1 | 107.3 | 3.6 | 0.1 | 71.3 | 7.4 | 0.1 | 101.9 | 13.7 | |||
Metribuzin | 0.02 | 101.2 | 1.4 | Simazine | 0.02 | 107.6 | 3.6 | Fipronil | 0.02 | 99.1 | 7.0 |
0.05 | 108.8 | 4.0 | 0.05 | 110.4 | 3.9 | 0.05 | 106.1 | 8.4 | |||
0.1 | 108.4 | 5.7 | 0.1 | 109.9 | 5.0 | 0.1 | 105.4 | 5.0 | |||
Norflurazon | 0.02 | 103.8 | 1.5 | S-Metolachlor | 0.02 | 107.2 | 4.1 | Fipronil Amide | 0.02 | 106.5 | 3.4 |
0.05 | 107.3 | 4.0 | 0.05 | 110.2 | 5.0 | 0.05 | 109.0 | 3.9 | |||
0.1 | 107.9 | 4.9 | 0.1 | 109.9 | 4.8 | 0.1 | 109.3 | 7.6 | |||
Oryzalin | 0.02 | 108.8 | 2.5 | Sulfoxaflor | 0.02 | 105.3 | 4.7 | Fipronil Sulfide | 0.02 | 99.4 | 5.2 |
0.05 | 102.7 | 12.4 | 0.05 | 107.4 | 7.2 | 0.05 | 104.5 | 7.6 | |||
0.1 | 102.9 | 6.7 | 0.1 | 106.1 | 6.5 | 0.1 | 102.6 | 6.1 | |||
Oxadiazon | 0.02 | 94.5 | 3.0 | Tebuconazole | 0.02 | 101.1 | 6.2 | Fipronil Sulfone | 0.02 | 105.1 | 4.8 |
0.05 | 98.2 | 5.9 | 0.05 | 106.4 | 7.4 | 0.05 | 107.6 | 4.3 | |||
0.1 | 96.9 | 8.8 | 0.1 | 104.1 | 7.0 | 0.1 | 105.1 | 5.2 | |||
Prometon | 0.02 | 110.8 | 2.6 | Tebufenozide | 0.02 | 107.0 | 2.3 | Desulfinyl Fipronil | 0.02 | 104.2 | 5.0 |
0.05 | 112.9 | 4.1 | 0.05 | 109.1 | 3.7 | 0.05 | 108.9 | 5.0 | |||
0.1 | 111.7 | 1.8 | 0.1 | 109.8 | 4.7 | 0.1 | 109.1 | 5.2 | |||
Prometryn | 0.02 | 93.5 | 3.9 | Tebuthiuron | 0.02 | 105.7 | 4.0 | Desulfinyl Fipronil Amide | 0.02 | 104.4 | 4.8 |
0.05 | 103.4 | 7.7 | 0.05 | 111.0 | 4.0 | 0.05 | 111.3 | 7.6 | |||
0.1 | 105.2 | 6.1 | 0.1 | 108.9 | 3.6 | 0.1 | 109.2 | 5.1 | |||
Propanil | 0.02 | 104.3 | 2.0 | Thiacloprid | 0.02 | 105.7 | 2.5 | ||||
0.05 | 109.6 | 2.9 | 0.05 | 110.5 | 4.0 | ||||||
0.1 | 109.5 | 3.1 | 0.1 | 108.6 | 4.5 | ||||||
Propargite NH4 | 0.02 | 76.4 | 6.5 | Thiamethoxam | 0.02 | 88.1 | 4.8 | ||||
0.05 | 78.4 | 9.3 | 0.05 | 89.2 | 11.7 | ||||||
0.1 | 76.0 | 11.7 | 0.1 | 87.8 | 7.3 |
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Nakhjavan, B.; Bland, J.; Khosravifard, M. Optimization of a Multiresidue Analysis of 65 Pesticides in Surface Water Using Solid-Phase Extraction by LC-MS/MS. Molecules 2021, 26, 6627. https://doi.org/10.3390/molecules26216627
Nakhjavan B, Bland J, Khosravifard M. Optimization of a Multiresidue Analysis of 65 Pesticides in Surface Water Using Solid-Phase Extraction by LC-MS/MS. Molecules. 2021; 26(21):6627. https://doi.org/10.3390/molecules26216627
Chicago/Turabian StyleNakhjavan, Bahar, Jason Bland, and Maryam Khosravifard. 2021. "Optimization of a Multiresidue Analysis of 65 Pesticides in Surface Water Using Solid-Phase Extraction by LC-MS/MS" Molecules 26, no. 21: 6627. https://doi.org/10.3390/molecules26216627