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PANG ET AL.: JOURNAL OF AOAC INTERNATIONAL VOL. 92,8 NO. 3,8 2009 S2716
Table 3.8 (3c3o8n7t9i6n7ue5d4)4

No.

Pesticide

Retention
time, min

Quantifying for MRM transitions for

precursor/
precursor/
product ion
product ion

Declustering
potential, V

Collision
energy, V

Collision
cell exit
potential, V

No.

Pesticide

time, min

product ion

product ion

potential, V

energy, V

potential, V

178
179

Spinosad
Fensulfothion

14.14
14.20

732/142
309/157

732/142; 732/98
309/157; 309/173

48
35

45; 96
33; 31

2; 2
3; 2

180

Dimethametryn

14.69

256/186

256/186; 256/96

36

28; 20

2; 2

181

Propanil

15.77

218/162

218/162; 218/127

45

23; 41

2; 2

182

Triticonazole

16.10

318/70

318/70; 318/125

28

42; 50

2; 3

183

Fluridone

16.22

330/309

330/309; 330/259

54

47; 61

3; 5

184

Prochloraz

16.31

376/308

376/308; 376/266

31

17; 22

5; 4

185
186

Methfuroxam
Benoxacor

16.79
17.35

230/137
260/149

230/137; 230/111
260/149; 260/134

32
40

27; 20
23; 41

3; 2
4; 2

187

Ethoxysulfuron

17.42

399/261

399/261; 399/218

60

21; 33

3; 3

188

Epoxiconazole

14.82; 17.84

330/121

330/121; 330/141

32

32; 25

2; 2

189

Fluquinconazole

18.39

376/349

376/349; 376/307

53

26; 32

9; 4

190

Mepanipyrim

18.86

224/77

224/77; 224/106

40

55; 36

2; 2

191

Methoxyfenozide

19.31

369/149

369/149; 369/313

19

25; 10

5; 5

192
193

Mepronil
Oryzalin

19.48
19.84

270/119
347/288

270/119; 270/228
347/288; 347/198

28
38

31; 20
24; 40

2; 3
2; 2

194

Fenoxycarb

20.03

302/116

302/116; 302/88

26

17; 31

2; 2

195

Thenylchlor

20.23

324/127

324/127; 324/99

30

24; 45

2; 2

196

Ditalimfos

20.34

300/148

300/148; 300/130

40

19; 42

2; 2

197

Fluorochloridone

20.52

312/292

312/292; 312/212

49

28; 43

5; 3

198

Etridiazol

21.58

247/219

247/219; 247/183

30

18; 26

3; 3

199
200

Butafenacil
Pyrimitate

21.65
21.75

475/331
306/170

475/331; 475/349
306/170; 306/154

50
35

27; 14
27; 28

4; 7
3; 2

201

Bromobutide

21.83

312/194

312/194; 312/119

35

18; 26

2; 2

202

Fenoxanil

21.83; 22.05

329/302

329/302; 329/189

38

16; 35

3; 2

203

Monalide

20.15; 21.98

240/85

240/85; 240/93

39

27; 53

2; 3

204

Kresoxim-methyl

22.29

314/235

314/235; 314/222

15

20; 18

3; 2

205

Quinalphos

22.37

299/163

299/163; 299/147

34

33; 31

2; 2

206

Benzoylprop-ethyl

23.71

366/105

366/105; 366/320

25

30; 13

2; 4

207

Coumaphos

24.39

363/227

363/227; 363/307

63

34; 25

4; 4

208

Phosalone

24.93

368/182

368/182; 368/111

31

23; 59

2; 2

209

Phoxim

24.95

299/97

299/97; 299/129

36

35; 18

2; 3

210

Piperophos

25.17

354/171

354/171; 354/143

26

30; 43

3; 2

211

Chlorphoxim

25.50

333/97

333/97; 333/163

22

34; 20

2; 2

212

MCPA-butoxyethyl ester

25.95

301/227

301/227; 301/155

43

8; 30

5; 2

213

Fluoroglycofen-ethyl

26.41

465/344

465/344; 465/223

47

21; 50

4; 2

214

Piperonyl butoxide

26.55

356/177

356/177; 356/119

15

19; 50

2; 2

215

Dithiopyr

26.62

402/354

402/354; 402/296

38

24; 35

5; 2

216

Flumiclorac-pentyl

27.00

441/308

441/308; 441/252

45

36; 51

3; 3

217

Oxyfluorfen

27.21

362/316

362/316; 362/237

32

18; 30

5; 2

218

Butachlor

27.25

312/238

312/238; 312/147

22

13; 46

2; 2

219

Iodofenphos

27.38

412/125

412/125; 412/287

43

30; 37

2; 10

220

Temephos

27.61

467/419

467/419; 467/341

40

27; 41

5; 4

221

Pendimethalin

27.85

282/212

282/212; 282/194

23

17; 25

2; 2

222

Fenpyroximate

28.38

422/366

422/366; 422/214

33

23; 38

6; 5

S2727 PANG ET AL.: JOURNAL OF AOAC INTERNATIONAL VOL. 92,8 NO. 3,8 2009
Table 3.8

(3c3o8n7t9i6n7ue5d4)4
Quantifying for MRM transitions for
precursor/
precursor/
product ion
product ion

Declustering
potential, V

Collision
energy, V

Collision
cell exit
potential, V

329/133; 329/143

39

25; 26

2; 5

350/125; 350/97

35

23; 42

2; 2

365/147

365/147; 365/309

65

37; 19

2; 3

29.74

379/115

379/115; 379/97

27

46; 82

4; 2

29.89

411/71

411/71; 411/313

48

29; 17

2; 5

Pesticide

Retention
time, min

223

Pyrethrin

28.70

329/133

224

Fenpropathrin

29.20

350/125

225

Pyridaben

29.62

226

Aspon

227

Spirodiclofen

No.

228

Leptophos

30.09

411/171

411/171; 411/379

51

30; 23

7; 16

229

Phenothrin

30.78; 30.98

351/183

351/183; 351/333

45

30; 14

3; 5

D group
230

Cyromazine

2.24

167/125

167/125; 167/108

46

25; 29

6; 6

231

Thiofanox sulfoxide

2.31

235/104

235/104; 235/178

16

13; 9

2; 3

232

Propamocarb

1.82; 2.33

189/102

189/102; 189/144

22

24; 17

3; 5

233

Ethirimol

2.36

210/140

210/140; 210/98

46

30; 39

2; 2

234

Dazomet

8.86

163/90

163/90; 163/120

27

12; 15

3; 3

235

Dicrotophos

9.23

238/112

238/112; 238/127

18

18; 24

2; 2

236

Metamitron

10.02

203/175

203/175; 203/104

33

22; 35

5; 3

237

Crimidine

10.04

172/136

172/136; 172/107

37

27; 30

4; 5

238

Dimethoate

10.55

230/199

230/199; 230/125

19

11; 28

3; 1.5

239

Terbumeton

10.73

226/170

226/170; 226/114

34

25; 34

3; 4

240

Desmetryn

10.79

214/172

214/172; 214/82

48

23; 45

4; 3

241

Imazalil

11.03

297/159

297/159; 297/255

45

36; 25

2; 3

241

Imazalil

11.03

297/159

297/159; 297/255

45

36; 25

2; 3

242

Hexazinone

11.43

253/171

253/171; 253/85

32

23; 45

3; 3

243

Carbetamide

11.50

237/192

237/192; 237/118

18

11; 18

2; 4

244

Dodemorph

11.58; 11.76

282/116

282/116; 282/98

29

30; 40

2; 2

245
246

Triamiphos
Chlorotoluron

11.90
13.30

295/135
213/72

295/135; 295/110
213/72; 213/140

47
29

34; 55
38; 33

2; 5
3; 3

247

Carbaryl

13.50

202/145

202/145; 202/127

20

15; 40

2; 2

248

Fluometuron

13.51

233/72

233/72; 233/160

29

40; 39

2; 4

249

Fosthiazate

13.51

284/104

284/104; 284/228

22

34; 13

2; 3

250

4,4-Dibromobenzophenone

13.55

339/283

339/283; 339/121

63

25; 44

2; 3

251

Isoproturon

13.84

207/72

207/72; 207/165

27

35; 19

2; 2

252
253

Carboxin
Fenfuram

13.90
14.24

236/143
202/109

236/143; 236/124
202/109; 202/120

37
38

22; 31
34; 21

2; 2
2; 2

254

Norflurazon

14.39

304/284

304/284; 304/160

66

27; 41

6; 5

255

3,4,5-Trimethacarb

14.65

194/137

194/137; 194/122

18

16; 37

2; 4

256

Nuarimol

14.99

315/81

315/81; 315/252

50

47; 31

2; 3

257

Diphenamid

15.22

240/134

240/134; 240/167

35

32; 31

2; 6

258

Buturon

15.52

237/84

237/84; 237/126

39

24; 40

2; 2

259
260

Thionazin
Benodanil

15.74
15.82

249/97
324/231

249/97; 249/221
324/231; 324/203

22
50

43; 12
30; 47

3; 2
6; 2

261

Cyproconazole

16.22

292/70

292/70; 292/125

38

45; 42

2; 4

262

Fenobucarb

16.34

208/95

208/95; 208/152

36

26; 12

2; 2

263

Methacrifos

16.88

241/125

241/125; 241/209

20

27; 12

2; 2

264

Simeconazole

16.96

294/70

294/70; 294/135

59

39; 30

2; 4

265

Anilazine

16.98

275/155

275/155; 275/169

33

34; 33

3; 6

266

Crufomate

17.26

292/236

292/236; 292/108

46

24; 40

4; 4

PANG ET AL.: JOURNAL OF AOAC INTERNATIONAL VOL. 92,8 NO. 3,8 2009 S2738
Table 3.8 (3c3o8n7t9i6n7ue5d4)4
Quantifying for MRM transitions for
precursor/
precursor/
product ion
product ion

Pesticide

Retention
time, min

267

Aziprotryne

17.53

226/156

268

Azoxystrobin

17.70

404/372

269

Triadimefon

18.00

294/197

No.

Declustering
potential, V

Collision
energy, V

Collision
cell exit
potential, V

226/156; 226/198

20

19; 13

3; 2

404/372; 404/344

32

20; 33

6; 3

294/197; 294/225

29

20; 17

2; 2

270

Ethoprophos

18.08

243/131

243/131; 243/97

33

27; 46

3; 3

271

Pyridaphenthion

18.32

341/189

341/189; 341/205

46

28; 26

2; 3

272

Coumatetralyl

18.63

293/175

293/175; 293/91

58

29; 56

3; 3

273

Trietazine

19.22

230/99

230/99; 230/132

40

32; 30

3; 2

274

Isoprothiolane

19.82

291/189

291/189; 291/231

13

28; 15

2; 3

275

Tebutam

19.91

234/91

234/91; 234/192

54

40; 21

1.5; 3

276

Triflumizole

20.12

346/278

346/278; 346/69

15

13; 30

5; 2

277

Flufenacet

20.53

364/194

364/194; 364/152

11

17; 27

7; 6

278

Propetamphos

20.66

282/156

282/156; 282/110

30

15; 40

2; 3

279

EPTC

21.32

190/128

190/128; 190/86

20

15; 18

3; 3

280

Tebufenozide

21.36

353/133

353/133; 353/297

46

30; 11

2; 2

281

Chlorfenvinphos

21.36

359/99

359/99; 359/155

27

45; 18

3; 2

282

Mecarbam

21.70

330/199

330/199; 330/171

19

20; 24

7; 7

283

Difenoconazole

22.50

406/251

406/251; 406/337

40

35; 23

4; 5

284

Tri-iso-butyl phosphate

22.60; 23.01

267/155

267/155; 267/211

24

12; 9

2; 2

285
286

Pyraclofos
Bensulide

22.98
23.45

361/257
398/158

361/257; 361/275
398/158; 398/314

43
21

30; 28
33; 14

5; 2
2; 5

287

Sulfallate

23.55

224/88

224/88; 224/116

25

30; 17

2; 1.5

288

Thiobencarb

24.08

258/125

258/125; 258/89

31

31; 71

3; 2

289

Mefenpyr-diethyl

24.35

373/160

373/160; 373/186

25

45; 50

3; 1.5

290

Pencycuron

24.49

329/125

329/125; 329/218

35

40; 20

1.5; 3

291

Vernolate

24.51

204/128

204/128; 204/162

22

16; 20

3; 6

292
293

Sulfotep
Profenefos

24.66
25.28

323/115
373/302.9

323/115; 323/171
373/302.9; 373/345

25
34

41; 20
24; 17

2; 2
3; 5

294

4,4-Dichlorobenzophenone

25.43; 26.42

251/139

251/139; 251/111

32

25; 52

2; 4

295

Isofenphos

25.69

346/121

346/121; 346/245

18

54; 18

2; 3

296

Clomeprop

25.88

324/120

324/120; 324/203

47

27; 21

4; 2

297

Kadethrin

26.93

397/171

397/171; 397/143

33

19; 35

3; 1.5

298

Sethoxydim

27.09

328/178

328/178; 328/282

40

28; 16

2; 3

299
300

Terbufos
Lactofen

27.42
27.59

289/103
462/344

289/103; 289/187
462/344; 462/223

20
64

14; 19
17; 42

4; 2
14; 9

301

Tebupirimfos

27.66

319/153

319/153; 319/277

34

42; 20

1.5; 4

302

Chlorpyrifos

27.87

350/198

350/198; 350/97

31

28; 46

3; 2

303

Ethion

28.17

385/143

385/143; 385/199

19

35; 12

3; 2

304

Sulprofos

28.31

323/219

323/219; 323/155

42

24; 32

2; 1.5

305

Butralin

28.62

296/240

296/240; 296/222

20

19; 30

4; 4

306

Bromophos-ethyl

29.86

393/337

393/337; 393/162

35

25; 52

3; 2

E group

E group
307

Mepiquat chloride

2.02

114/98

114/98; 114/84

38

37; 39

2; 2

308

Dimethirimol

2.37; 9.39

210/140

210/140; 210/98

42

29; 35

2; 3

309

2,6-Dichlorobenzamide

9.55

190/173

190/173; 190/145

44

31; 36

2; 6

310

Atratone

10.03

212/170

212/170; 212/100

30

28; 36

6; 2

839 Pesticide and Chemical Contaminant Multiresidues in Animal Muscles by GPC Cleanup GCMS and LCMS

Table 3.8

(3c3o8n7t9i6n7ue5d4)4
Quantifying for MRM transitions for
precursor/
precursor/
product ion
product ion

No.

Pesticide

Retention
time, min

311

Isocarbamid

10.11

186/87

312

Chloridazon

10.33

222/104

Declustering
potential, V

Collision
energy, V

Collision
cell exit
potential, V

186/87; 186/130

25

25; 16

3; 2

222/104; 222/92

43

31; 37

2; 3

313

Dioxacarb

10.54

224/123

224/123; 224/167

15

22; 11

3; 3

314

Tricyclazole

10.71

190/136

190/136; 190/163

42

38; 31

2; 2

315

Flumetsulam

10.99

326/129

326/129; 326/262

44

40; 25

2; 2

316

Triazoxide

11.54

248/150

248/150; 248/124

47

48; 45

2; 2

317

Ametryn

11.90

228/96

228/96; 228/158

35

36; 32

2; 5

318

Allidochlor

12.09

174/98

174/98; 174/106

27

14; 15

3; 2

319

Fenpropidin

11.90

274/147

274/147; 274/165

46

38; 46

5; 2

320

Azamethiphos

12.22

325/183

325/183; 325/112

26

21; 51

3; 2

321

Lenacil

12.35

235/153

235/153; 235/136

26

25; 46

2; 2

322

Cinosulfuron

12.50

414/183

414/183; 414/157

39

28; 34

2; 3

323

Metribuzin

12.56

215/187

215/187; 215/171

37

23; 27

3; 5

324

Pyrifenox

12.97

295/93

295/93; 295/263

43

42; 25

2; 2

325

Terbutryn

13.45

242/186

242/186; 242/91

35

25; 37

2; 2

326

Alanycarb

13.57

339/283

339/283; 339/175

68

21; 32

12; 2

327

Dimethylaminosulfotoluidide (DMST)

13.61

215/106

215/106; 215/151

35

19; 11

3; 3

328

Azaconazole

13.72

300/159

300/159; 300/231

35

40; 23

2; 4

329

Atrazine

13.79

216/174

216/174; 216/104

33

24; 40

2; 3

330

Cyprazine

13.80

228/186

228/186; 228/108

48

24; 37

2; 3

331
332

Heptanophos
Bensulfuron-methyl

14.31
14.84

251/127
411/149

251/127; 251/89
411/149; 411/182

30
29

20; 49
31; 30

2; 2
2; 2

333

Dipropetryn

14.90

256/144

256/144; 256/172

39

37; 30

4; 2

334

Metazachlor

14.91

278/134

278/134; 278/210

15

21; 14

3; 2

335

Iodosulfuron-methyl

15.41

530/390

530/390; 530/163

34

21; 22

4; 2

336

Dimethomorph

15.14; 15.56

388/301

388/301; 388/165

40

28; 45

3; 2

337

Sebutylazine

15.60

230/174

230/174; 230/104

37

25; 42

2; 2

338
339

Bupirimate
Phorate sulfone

15.92
16.13

317/108
293/143

317/108; 317/210
293/143; 293/171

37
31

36; 30
24; 14

4; 2
2; 4

340

Metosulam

16.65

418/175

418/175; 418/190

62

40; 38

2; 2

341

Pyrazosulfuron-ethyl

16.83

415/182

415/182; 415/369

26

31; 17

2; 3

342

Diethofencarb

16.89

268/152

268/152; 268/180

17

29; 22

3; 3

343

Azinphos-methyl

16.90

318/132

318/132; 318/261

19

21; 10

2; 10

344

Linuron

16.92

249/160

249/160; 249/182

32

25; 21

2; 2

345
346

Uniconazole
Phosmet

17.32
17.51

292/70
318/160

292/70; 292/125
318/160; 318/133

44
22

47; 46
20; 48

2; 2
5; 4

347

Mefenacet

17.85

299/120

299/120; 299/148

23

36; 23

2; 2

348

Tetraconazole

18.35

372/159

372/159; 372/150

41

44; 46

6; 4

349

Tebuconazole

18.46

308/70

308/70; 308/125

45; 55

2; 3

350

Propyzamide

18.50

256/190

256/190; 256/173

/7257
36

20; 32

2; 2

351

Methyl parathion

18.67

264/232

264/232; 264/250

33

20; 18

3; 5

352

Hexaconazole

19.06

314/70

314/70; 314/159

34

45; 45

3; 6

353

Metolachlor

19.93

284/252

284/252; 284/176

34

22; 36

3; 2

354

Malathion

19.93

331/127

331/127; 331/99

30

18; 35

2; 2

355

Alachlor

20.17

270/238

270/238; 270/162

29

14; 25

3; 2

23

gpc-gcms
GPC-GCMS

GPC-GCMS

GPCGCMS

GPC
GCMS
GCMS

PROG110

PANG ET AL.: JOURNAL OF AOAC INTERNATIONAL VOL. 92,8 NO. 3,8 2009 S275
Table 3.8 (3c3o8n7t9i6n7ue5d4)4
Quantifying for MRM transitions for
precursor/
precursor/
product ion
product ion

Declustering
potential, V

Collision
energy, V

Collision
cell exit
potential, V

326/70; 326/159
252/170; 252/110

34
23

50; 45
17; 31

3; 3
3; 2

314/120; 314/162

32

40; 22

2; 2

346/304

346/304; 346/262

27

20; 25

4; 2

231/157

231/157; 231/101

25

10; 21

2; 2

No.

Pesticide

Retention
time, min

356
357

Diniconazole
Furmecyclox

20.31
20.99

326/70
252/170

358

Isazofos

21.72

314/120

359

Nitralin

22.39

360

Dibutyl succinate

22.60

Validation study

S2749 PANG ET AL.: JOURNAL OF AOAC INTERNATIONAL VOL. 92,8 NO. 3,8 2009

360

Dibutyl succinate

22.60

231/157

231/157; 231/101

25

10; 21

2; 2

361

Picoxystrobin

22.97

368/145

368/145; 368/205

21

27; 12

3; 3

362

Tri-n-butyl phosphate

23.07

267/99

267/99; 267/155

41

24; 14

3; 2

363

Cadusafos

23.29

271/159

271/159; 271/97

27

14; 36

2; 3

364

Phenthoate

23.56

321/135

321/135; 321/163

20

26; 15

2; 2

365

Cartap hydrochloride

23.87

238/210

238/210; 238/117

30

25; 30

2; 3

366

alpha-HCH

23.93

306/164

306/164; 306/108

40

28; 41

2; 2

367

Pyraclostrobin

24.10

388/194

388/194; 388/163

19; 29

7; 7

368

Thiazopyr

24.23

397/335

397/335; 397/275

48

42; 51

5; 9

369

Pebulate

24.54

204/128

204/128; 204/176

27

15; 15

4; 4

370

Prohydrojasmon

24.55

255/97

255/97; 255/195

35

36; 17

3; 2

371

Cycloate

24.60

216/83

216/83; 216/134

28

24; 18

2; 2

372

Prallethrin

25.24

301/105

301/105; 301/133

27

29; 17

2; 2

373

Methiocarb

16.34

226/121

226/121; 226/169

19

25; 12

2; 2

374

EPN

25.76

324/157

324/157; 324/296

41

34; 19

4; 2

375

Prosulfocarb

25.88

252/91

252/91; 252/128

29

38; 15

2; 2

376

Pirimiphos methyl

23.92

306/108

306/108; 306/95

42

42; 50

3; 3

377

Benfluralin

28.12

336/57

336/57; 336/236

45

30; 20

3; 3

378

Isopropalin

29.67

310/226

310/226; 310/208

30

27; 31

2; 2

379

Etofenprox

31.11

394/135

394/135; 394/359

11

35; 14

2; 6

minicolumns. Highly pigmented samples were cleaned up

with class-9specific SPE columns. The concentrated extracts
were analyzed by selective detection with GC or LC.
Lott and Barker (528)6 proposed a multiresidue technique
using matrix solid-9phase dispersion (5MSPD)6 for isolation of
14 chlorinated pesticides from crayfish hepatopancreas.
Samples were blended with 2 g C18 sorbent. The
C18/hepatopancreas matrix blend and 2 g activated Florisil
were used as an extraction column from which the pesticides
were eluted by adding 8 mL acetonitrile. A 2 L amount of the
eluate was directly analyzed by GC-9ECD.
Bordet et al. (529)6 conducted an interlaboratory study to
validate a GC method for determination of 21 organochlorine
pesticides,8 6 pyrethroid pesticides,8 and 7 PCB congeners in
milk,8 beef fat,8 fish,8 and eggs. The method was performed at
low contamination levels,8 which represent relevant contents
in food,8 and it is an extension of the European standard
(5Method NF-9EN-91528,8 Parts 1-94)6. It enlarges the applicable
scope of the reference EN method to pyrethroid pesticides and
proposes the use of SPE as a cleanup procedure. Cryogenic
extraction was made,8 and SPE cleanup was performed with

2 successive SPE cartridges: C18 and Florisil. Residues were

measured by GC-9ECD.
Rimkus etsilica
al. (530)6
used GPC
cleanup andautomated
subsequent
conventional
gel column
chromatography
by
an online solvent evaporation of the GPC fraction,8 followed
by normal phase LC separation,8 for multiresidue analysis of
fats. The ternary solvent system n-9hexanetolueneacetone
(588 +7 10 +7 2)6 was used as the mobile phase,8 which resulted in
only one HPLC fraction for all relevant analytes. The HPLC
column was cleaned automatically after each sample by
backflushing with polar solvents.
On the basis of this literature (5630)6,8 GPC cleanup,8
GC/MS,8 and LC/MS/MS determination methods for
437 pesticides in animal muscles were established in
20042005 (531,8 32)6. After 2006,8 the authors conducted a
detailed study on the pesticide multiresidues in animal
muscles,8 enabling an increase in pesticides analyzed by
GC/MS from 368 to 478. Thereafter,8 the authors appraised the
LC/MS/MS behaviors of 766 pesticides and established an
LC/MS/MS data bank for 465 pesticides,8 enabling
LC/MS/MS analysis of pesticides to achieve a substantiative

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81

90

2014

~
240

2014 Baidu