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Pesticides Standards for JP Water Quality

FUJIFILM Wako Pure Chemical provides many types of standards for residual pesticide analysis. In the amendment of the Japanese Waterworks Act on March 28, 2013, the classification of pesticide related compounds was reviewed and 120 pesticides were added to the measurement list. In the conventional methods, GC/MS or LC/MS assay tests are carried out after pretreatment by solid phase extraction (SPE). In the new method, simultaneous analysis is introduced as an efficient method and applied to 195 kinds of pesticide related compounds listed on appendix of 20th revised on March 28, 2018. Several types of mixed pesticide standard solutions that are listed on the Water Supply Act in Japan are available.

Abbreviation List

  • WQ1: 66 Pesticides Mixture Standard Solution WQ-1-2
  • WQ2: 15 Pesticides Mixture Standard Solution WQ-2
  • WQ3: 28 Pesticides Mixture Standard Solution WQ-3
  • WQ4: 63 Pesticides Mixture Standard Solution WQ-4
  • WQ5: 48 Pesticides Mixture Standard Solution WQ-5
  • WQ6: Pesticides Mixture Standard Solution WQ-6
  • WQ7: Pesticides Mixture Standard Solution WQ-7
  • WQ8: Pesticides Mixture Standard Solution WQ-8
  • WQ9: 29 Pesticides Mixture Standard Solution WQ-9

WQ1,WQ2

66 Pesticides Mixture Standard Solution WQ-1-2 (each 20μg/ml Acetone Solution)

GC/MS Chromatogram*

00339_img08.png
Peak No. Constituent Monitoring Ions
(m/z)
Peak No. Constituent Monitoring Ions
(m/z)
Peak No. Constituent Monitoring Ions
(m/z)
1 Dichlorvos (DDVP) 79 109 185 23 Alachlor 188 160 146 45 Flutolanil 173 145 281
2 Trichlorfon (DEP) (deg.) 109 75 185 24 Tolclofos-methyl 265 125 250 46 Napropamide 72 128 100
3 Dichlobenil (DBN) 171 100 173 25 Dithiopyr 354 306 286 47 Pretilachlor 176 238 262
4 Etridiazole (Echlomezol) 211 183 213 26 Metalaxyl 160 206 132 48 Isoprothiolane 118 189 290
5 Chloroneb 191 193 206 27 Simetryn 213 170 155 49 Buprofezin 105 175 106
6 Isoprocarb (MIPC) 121 136 122 28 Fenitrothion (MEP) 277 260 125 50 Isoxathion 105 177 313
7 Molinate 126 98 188 29 Malathion (Malathon) 127 173 93 51 Mepronil 119 269 91
8 Fenobucarb (BPMC) 121 208 150 30 Esprocarb 91 222 162 52 Chlornitrofen (CNP) 317 319 289
9 Trifluralin 306 264 290 31 Chlorpyrifos 197 199 314 53 Propiconazole 259 173 261
10 Benfluralin (Bethrodine) 292 264 276 32 Thiobencarb (Benthiocarb) 100 72 125 54 Edifenphos (EDDP) 109 173 310
11 Pencycuron 125 180 127 33 Fenthion (MPP) 278 153 125 55 Thenylchlor 127 288 141
12 Dimethoate 87 125 93 34 Fthalide 243 241 215 56 Pyributicarb 165 108 181
13 Simazine (CAT) 201 186 173 35 Pendimethalin 252 191 281 57 Pyridaphenthion 340 199 125
14 Atrazine 200 215 173 36 Isofenphos 213 121 185 58 Iprodione 314 316 187
15 Diazinon 179 137 304 37 Dimethametryn 212 255 240 59 Piperophos 122 140 320
16 Propyzamide 173 145 175 38 Methyldymron 107 119 91 60 EPN 157 169 185
17 Pyroquilon 173 130 144 39 Phenthoate (PAP) 274 125 93 61 Anilofos 226 125 228
18 Disulfoton (Ethylthiomethon) 89 97 186 40 Procymidone 283 96 285 62 Bifenox 341 310 343
19 Chlorothalonil (TPN) 266 264 268 41 Dimepiperate 119 145 91 63 Pyriproxyfen 136 226 137
20 Iprobenfos (IBP) 204 246 42 Captan 79 149 117 64 Mefenacet 192 120 136
21 Terbucarb (MBPMC) 205 220 206 43 Methidathion (DMTP) 145 85 302 65 Cafenstrole 100 188 167
22 Bromobutide 119 232 120 44 Butamifos 286 258 200 66 Etofenprox 163 135 183
  • Analysis conditions, charts, and detected ions are reference data. It is not the data to guarantee the pesticide mixed standard solution.

Analysis conditions

[ Instrument ]

Shimadzu QP-2010 Ultra

[ GC ]

Column BPX5 0.25 μm, 0.25 mm × 30 m

Column temperature 50 ℃ (2 min)→10 ℃/min→220 ℃→2.5 ℃/min→270 ℃→10 ℃/min→300 ℃ (5 min)

Injection temperature 220 ℃

Carrier gas He 2.0 mL/min

Splitless 2 min

[ MS ]

Ionization EI

Interface temperature 250 ℃

15 Pesticides Mixture Standard Solution WQ-2 (each 20μg/ml Acetone Solution)

GC/MS Chromatogram*

00339_img09.png
Peak No. Constituent Monitoring Ions (m/z) Peak No. Constituent Monitoring Ions (m/z)
1 Diazinon Oxon 137 273 288 9 Isoxathion Oxon 161 105 125
2 Tolclofos-methyl Oxon 249 109 251 10 MPP Oxon Sulfoxide 262 278 247
3 MEP Oxon 244 109 261 11 MPP Oxon Sulfone 294 109 215
4 Malaoxon 127 195 99 12 MPP Sulfoxide 278 125 294
5 MPP Oxon 262 109 247 13 MPP Sulfone 310 125 231
6 Chlorpyrifos Oxon 270 242 298 14 Benzoepin Sulfate 272 274 229
7 Isofenphos Oxon 229 201 314 15 EPN Oxon 141 169 306
8 Butamifos Oxon 244 216 287
  • Analysis conditions, charts, and detected ions are reference data. It is not the data to guarantee the pesticide mixed standard solution.

Analysis conditions

[ Instrument ]

Shimadzu QP-2010 Ultra

[ GC ]

Column BPX5 0.25 μm, 0.25 mm × 30 m

Column temperature 80 ℃ (1 min)→15 ℃/min→170 ℃→3 ℃/min→200 ℃→10 ℃/min→300 ℃ (3 min)

Injection temperature 220 ℃

Carrier gas He 1.8 mL/min

Splitless 1 min

[ MS ]

Ionization EI

Interface temperature 280 ℃

WQ3,WQ4

28 Pesticides Mixture Standard Solution WQ-3 (each 20μg/ml Acetonitrile Solution)

LC/MS Chromatogram*

00339_img10.png
Peak No. Constituent Monitoring Ions (m/z) Mode Peak No. Constituent Monitoring Ions (m/z) Mode
Precursor Product Precursor Product
1 Asulam 231.1 156.0 + 15 Flazasulfuron 408.2 182.0 +
2 Methomyl 163.1 88.0 + 16 Azoxystrobin 404.1 372.0 +
3 MPP Oxon Sulfoxide 279.1 263.9 + 17 Dymron 269.2 151.1 +
4 Tricyclazole 190.1 136.0 + 18 Iprodione 330.2 244.9 +
5 Thiodicarb 355.1 87.8 + 19 Carpropamid 334.1 139.1 +
6 MPP Oxon Sulfone 295.2 216.9 + 20 Fenthion (MPP) 279.2 168.9 +
7 MPP Sulfoxide 295.2 109.0 + 21 Diuron (DCMU) 233.2 71.9 -
8 Carbofuran 222.3 165.0 + 22 2,4-D (2,4-PA) 219.0 161.1 -
9 Thiram (Thiuram) 241.2 87.8 + 23 Triclopyr 253.9 196.1 -
10 Probenazole 224.1 41.1 + 24 Mecoprop (MCPP) 213.2 141.1 -
11 Bentazone 239.2 132.2 + 25 Siduron 277.2 45.1 -
12 MPP Oxon 263.1 230.9 + 26 Halosulfuron-methyl 433.1 252.1 -
13 Bensulfuron-methyl 411.1 149.0 + 27 Fipronil 437.0 332.0 -
14 MPP Sulfone 311.2 125.0 + 28 Bensulide 396.2 213.2 -
  • Analysis conditions, charts, and detected ions are reference data. It is not the data to guarantee the pesticide mixed standard solution.

Analysis conditions

[ Instrument ]

Shimadzu LCMS-8040

[ HPLC ]

Column Wakopak® Ultra C18-3 2.0 × 150 mm

Column temperature 40 ℃

Eluent A) 0.1 % HCOOH in H2O, B) CH3CN

Gradient

Time (min) B conc. (%)
0-30 0-100
30-35 100
35-35.01 100-0
35.01-45 0

Flow rate 0.2 mL/min

[ MS ]

Ionization ESI

Mode MRM

63 Pesticides Mixture Standard Solution WQ-4 (each 20μg/ml Acetonitrile Solution)*

LC/MS Chromatogram**

00339_img11.png
Peak No. Constituent Monitoring Ions (m/z) Mode Peak No. Constituent Monitoring Ions (m/z) Mode Peak No. Constituent Monitoring Ions (m/z) Mode
Precursor Product Precursor Product Precursor Product
1 Oxamyl 237 72 + 22 Simeconazole 294 70 + 43 Indanofan 341 175 +
2 Pymetrozine 218 105 + 23 Naproanilide 292 171 + 44 Diflubenzuron 311 158 +
3 Thiamethoxam 292 211 + 24 Tebufenozide 351 133 + 45 Tetrachlorvinphos
(CVMP)
367 127 +
4 Trinexapac-ethyl 253 69 + 25 Difenoconazole 406 251 + 46 Tebuconazole 308 70 +
5 Cinosulfuron 414 183 + 26 Triflumizole 346 278 + 47 Cyprodinil 226 108 +
6 Acetamiprid 223 126 + 27 Benzofenap 431 105 + 48 Fentrazamide 350 154 +
7 Thiacloprid 253 126 + 28 Quizalofop-ethyl 373 299 + 49 Etobenzanid 340 179 +
8 Pyrazosulfuron-ethyl 415 182 + 29 Oxaziclomefone 376 190 + 50 Oxadiargyl 358 341 +
9 Cyanazine 241 214 + 30 Dinotefuran 203 129 + 51 Phoxim 299 77 +
10 Bromacil 261 205 + 31 Nitenpyram 271 56 + 52 Pirimiphos-methyl 306 164 +
11 Bendiocarb 224 167 + 32 Monocrotophos 224 193 + 53 Pyrazolate 439 91 +
12 Ethoxysulfuron 399 261 + 33 Imidacloprid 256 209 + 54 Clomeprop 324 120 +
13 Furametpyr 334 157 + 34 Clothianidin 250 132 + 55 Pentoxazone 371 286 +
14 (E)-Metominostrobin 285 196 + 35 Metribuzin 215 49 + 56 Silafluofen 426 287 +
15 (Z)-Pyriminobac-methyl*** 362 330 + 36 Fluazifop 328 282 + 57 MCPA(MCP) 199 141 -
16 Ametryn 228 186 + 37 Linuron 249 182 + 58 Dichlorprop 233 161 -
17 (E)-Pyriminobac-methyl*** 362 330 + 38 Acibenzolar-S-methyl 211 136 + 59 Propanil(DCPA) 216 160 -
18 Cumyluron 303 185 + 39 Boscalid 343 307 + 60 Inabenfide 337 122 -
19 Cyproconazole 292 70 + 40 Benzobicyclon 447 257 + 61 Tiadinil 266 71 -
20 Prometryn 242 158 + 41 Diclomezine 255 141 + 62 Thifluzamide 527 125 -
21 Chromafenozide 395 175 + 42 Tetraconazole 372 159 + 63 Flusulfamide 413 171 -
64 Fluazinam 463 416 -

*This product contains 2% methanol.
**Analysis conditions, charts, and detected ions are reference data. It is not the data to guarantee the pesticide mixed standard solution.
***The preparation concentration is converted to 20 µg/mL as a total of E and Z isomer (each 10 μg/mL).

Analysis conditions

[ Instrument ]

Shimadzu LCMS-8040

[ HPLC ]

Column Wakopak® Ultra C18-3 2.0 × 75 mm

Column temperature 40 ℃

Eluent A) 5 mmol/L CH3COONH4 in H2O, B) 5 mmol/L CH3COONH4 in CH3OH

Gradient

Time (min) B conc. (%)
0-2 5
2-6 5-40
6-41 40-75
41-46 75-100
46-50 100
50-50.01 100-5
50.01-60 5

Flow rate 0.15 mL/min

[ MS ]

Ionization ESI

Mode MRM

WQ5,WQ6

48 Pesticides Mixture Standard Solution WQ-5 (each 20μg/ml Acetone Solution)

GC/MS Chromatogram*

00339_img12.png
Peak No. Constituent Monitoring Ions (m/z) Peak No. Constituent Monitoring Ions (m/z) Peak No. Constituent Monitoring Ions (m/z)
1 Propoxur (PHC) 110 152 18 Chlorthal-dimethyl (TCTP) 301 299 35 (E)-Pyriminobac-methyl*** 302 256
2 Cadusafos 159 158 19 Tetraconazole 336 338 36 Propargite (BPPS) 173 150
3 Cyanophos (CYAP) 243 109 20 Cyanazine 225 212 37 Tebuconazole 250 125
4 Dichlofenthion (ECP) 279 223 21 Quinoclamine (ACN) 207 172 38 Orysastrobin 116 205
5 Benfuresate 163 256 22 Fosthiazate 195 283 39 Acetamiprid 152 126
6 Chlorpyrifos-methyl
(Chlorpyrifosmethyl)
286 288 23 Cyprodinil 224 225 40 Cumyluron 267 120
7 Propanil (DCPA) 161 163 24 Thiamethoxam 212 182 41 Furametpyr 157 298
8 Simeconazole 121 73 25 Triflumizole 278 206 42 Indanofan 174 159
9 Metribuzin 198 144 26 Propaphos 220 304 43 Phosalone 182 367
10 Cinmethylin 105 123 27 Butachlor 176 160 44 Cyhalofop-butyl 256 229
11 Prometryn 241 184 28 Tetrachlorvinphos (CVMP) 329 331 45 Pyraclofos 360 194
12 Ametryn 227 212 29 Paclobutrazol 236 125 46 Etobenzanid 179 149
13 Pirimiphos-methyl 290 276 30 (E)-Metominostrobin 191 196 47 Boscalid 140 342
14 (E)-Dimethylvinphos** 295 297 31 Thifluzamide 194 449 48 Thiacloprid 126 101
15 Bromacil 205 207 32 Uniconazole P 234 236 49 Difenoconazole 323 265
16 Metolachlor 162 238 33 (Z)-Pyriminobac-methyl*** 302 256 50 Pyrazoxyfen 105 91
17 (Z)-Dimethylvinphos** 295 297 34 Cyproconazole 222 139

*Analysis conditions, charts, and detected ions are reference data. It is not the data to guarantee the pesticide mixed standard solution.
**The preparation concentration is converted to 20 µg/mL as a total of E and Z isomer (each 10 μg/mL).
***The preparation concentration is converted to 20 µg/mL as a total of E and Z isomer.

Analysis conditions

[ Instrument ]

Shimadzu QP-2010 Ultra

[ GC ]

Column BPX5 0.25 μm, 0.25 mm × 30 m

Column temperature 50 ℃ (1 min)→20 ℃/min→210 ℃→10 ℃/min→290 ℃ (5min)

Injection temperature 250 ℃

Carrier gas He 1.2mL/min

Splitless 1 min

[ MS ]

Ionization EI

Interface temperature 280℃

Pesticides Mixture Standard Solution WQ-6 (Ferimzone,Pyraclonil,Nereistoxin each 20μg/ml Methanol Solution)

GC/MS Chromatogram*

00339_img13.png
Peak No. Constituent Monitoring Ions (m/z) Mode Peak No. Constituent Monitoring Ions (m/z) Mode
Precursor Product Precursor Product
1 Nereistoxin** 150 105 + 3 (E)-Ferimzone*** 255 91 +
2 Pyraclonil 315 169 + 4 (Z)-Ferimzone*** 255 91 +

*Analysis conditions, charts, and detected ions are reference data. It is not the data to guarantee the pesticide mixed standard solution.
**The preparation concentration is converted to 20 µg/mL as a free base.
***The preparation concentration is converted to 20 µg/mL as a total of E and Z isomer. Ratios of isomer may change during storage.

Analysis conditions

[ Instrument ]

Shimadzu LCMS-8040

[ HPLC ]

Column Wakopak® Wakosil-Ⅱ 3C18HG 2.0 × 150 mm

Column temperature 40 ℃

Eluent A) 5 mmol/L CH3COONH4 in H2O, B) 5 mmol/L CH3COONH4 in CH3OH

Gradient

Time (min) B conc. (%)
0-25 50-70
25-30 70

Flow rate 0.2 mL/min

[ MS ]

Ionization ESI

Mode MRM

WQ7,WQ8

Pesticides Mixture Standard Solution WQ-7 (Iminoctadine,Diquat,Paraquat each 20μg/ml Water Solution)*

LC/MS Chromatogram**

00339_img14.png
Peak No. Constituent Monitoring Ions (m/z) Mode Peak No. Constituent Monitoring Ions (m/z) Mode Peak No. Constituent Monitoring Ions (m/z) Mode
Precursor Product Precursor Product Precursor Product
1 Iminoctadine
Triacetate, Albesilate
179 69 + 2 Diquat*** 183 157 + 3 Paraquat*** 185 170 +

*When weighing out this product, use a plastic ware made of polytetrafluoroethylene or polypropylene.
**Analysis conditions, charts, and detected ions are reference data. It is not the data to guarantee the pesticide mixed standard solution.
***The preparation concentration is converted to 20 µg/mL as a free base.

Analysis conditions

[ Instrument ]

Shimadzu LCMS-8040

[ HPLC ]

Column Wakopak® Wakosil-Ⅱ 5SIL-AQ 2.0 × 150 mm

Column temperature 40 ℃

Eluent HCOONH4 Buffer : CH3CN = 70 : 30

Flow rate 0.4 mL/min

[ MS ]

Ionization ESI

Mode MRM

Pesticides Mixture Standard Solution WQ-8 (Glyphosate,Glufosinate,AMPA each 20μg/ml Water Solution)*

LC/MS Chromatogram**

00339_img15.png
Peak No. Constituent Monitoring Ions (m/z) Mode Peak No. Constituent Monitoring Ions (m/z) Mode Peak No. Constituent Monitoring Ions (m/z) Mode
Precursor Product Precursor Product Precursor Product
1 Glyphosate 390 168 - 2 Glufosinate*** 402 180 - 3 AMPA ((Aminomethyl)phosphonic Acid) 332 110 -

*When weighing out this product, use a plastic ware made of polytetrafluoroethylene or polypropylene.
**Analysis conditions, charts, and detected ions are reference data. It is not the data to guarantee the pesticide mixed standard solution.
***The preparation concentration is converted to 20 µg/mL as a free base.

Analysis conditions

[ Instrument ]

Shimadzu LCMS-8040

[ HPLC ]

Column Wakopak® Ultra C18-5 4.6 × 150 mm

Column temperature 40 ℃

Eluent A) 5 mmol/L CH3COONH4 in H2O, B) CH3CN

Eluent

Time (min) B conc. (%)
0-15 30-100

Flow rate 0.5 mL/min

[ MS ]

Ionization ESI

Mode MRM

WQ9

29 Pesticides Mixture Standard Solution WQ-9 (each 20μg/mL Acetonitrile Solution)

LC/MS Chromatogram*

00339_img16.png
Peak No. Constituent Monitoring Ions (m/z) Mode Peak No. Constituent Monitoring Ions (m/z) Mode Peak No. Constituent Monitoring Ions (m/z) Mode
Precursor Product Precursor Product Precursor Product
1 Methamidophos 142 94 + 12 (Z)-Dimethylvinphos**** 333 127 + 23 Chlorpyrifosmethyl 324 125 +
2 Acephate 184 143 + 13 (5Z)-Orysastrobin*** 392 205 + 24 Cinmethylin 292 105 +
3 Amitraz Metabolite** 163 107 + 14 (E)-Dimethylvinphos**** 333 127 + 25 Butachlor 312 238 +
4 Tefuryltrione 460 262 + 15 Metolachlor 284 252 + 26 Tolfenpyrad 384 197 +
5 Quinoclamine (ACN) 208 105 + 16 Uniconazole P 292 70 + 27 Dichlofenthion (ECP) 315 259 +
6 Propoxur (PHC) 210 111 + 17 Fenoxanil 329 302 + 28 Cypermethrin 433 191 +
7 Carbaryl (NAC) 202 145 + 18 Propaphos 305 221 + 29 trans-Permethrin**** 408 183 +
8 Fosthiazate 284 104 + 19 Pyrazoxyfen 403 91 + 30 cis-Permethrin**** 408 183 +
9 Benfuresate 274 18 + 20 Pyraclofos 361 257 + 31 Cyanophos (CYAP) 228 118 -
10 Paclobutrazol 294 70 + 21 Phosalone 368 182 + 32 Ethiprole 395 331 -
11 Orysastrobin*** 392 205 + 22 Cadusafos 271 159 +

*Analysis conditions, charts, and detected ions are reference data. It is not the data to guarantee the pesticide mixed standard solution.
**The preparation concentration is converted to 20 µg/mL as a free base.
***The preparation concentration is converted to 20 µg/mL as a total of Orysastrobin and (5Z)-Orysastrobin (each 10 μg/mL).
****The preparation concentration is converted to 20 µg/mL as a total of E and Z isomer (each 10 μg/mL).

Analysis conditions

[ Instrument ]

Shimadzu LCMS-8040

[ HPLC ]

Column Wakopak® Wakosil-Ⅱ 3C18HG 2.0 × 150 mm

Column temperature 40 ℃

Eluent A) 5 mmol/L CH3COONH4 in H2O, B) 5 mmol/L CH3COONH4 in CH3OH

Eluent

Time (min) B conc. (%)
0-7 10-45
7-42 45-80
42-46 80-100
46-51 100

Flow rate 0.2 mL/min

[ MS ]

Ionization ESI

Mode MRM

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Author: T. Miura

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