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Comprehensive Pesticide Residue Analysis by LC-MS/MS Using an Ultra Aqueous C18 Column

By Becky Wittrig, Ph.D., Global HPLC Specialist, and André Schreiber, Ph.D., Applied Biosystems/MDS Analytical Technologies
  • Easily resolve and quantify more than 280 pesticide species.
  • Use LC/MS/MS to reliably monitor difficult polar and/or thermally unstable species.
  • Aqueous C18 phase offers optimal selectivity and retention.

Food safety is a topic of great interest globally. With recent contamination issues in a wide range of commodities, ensuring the quality of our food supply is becoming increasingly important. Pesticide residue content is one area of concern. While pesticides have typically been monitored by gas chromatography, polar and/or thermally unstable pesticides are difficult or impossible to monitor using this approach. Thus, traditional HPLC techniques are used for select pesticide classes, such as the carbamate and phenylurea pesticides.

Aqueous C18 columns offer greater retention of polar compounds than traditional C18 columns.

With recent advances in LC/MS/MS instrumentation, this technique is quickly gaining acceptance for pesticide residue testing. LC/MS/MS can be used to simultaneously monitor hundreds of potential contaminants—including those difficult to detect by GC. Using both LC/MS/MS and GC approaches allows for a faster, more complete picture of pesticide residues. MS/MS technology also permits identification of the target pesticides through the selection of specific MRM transitions for each compound. For example, aldicarb, a carbamate pesticide, uses two MRM transitions of 208.2->89.1amu and 208.2->116.1amu.

While the MS/MS detector allows for specific, sensitive detection of the pesticide species, the LC separation is still important to ensure the highest quality data. Conventional C18 stationary phases are typically used for pesticide monitoring, but the selectivity and retention is poor for more polar species. In contrast, Ultra Aqueous C18 columns are ideal for multi-pesticide residue monitoring methods. In Figure 1, the analysis of more than 280 pesticides using the 3µm Ultra Aqueous C18 is shown. Optimized stationary phase selectivity allows for an even distribution of the compounds throughout the retention time window (Tables I and II). As well, retention of more polar pesticides is greatly improved, as demonstrated in Figure 1C. The Ultra Aqueous C18 column, in a 100 x 2.1mm, 3µm configuration is the column of choice for LC/MS/MS pesticide monitoring methods.

Ultra-high pressure LC (UHPLC) can also be used with MS/MS detection for monitoring pesticide residues. UHPLC allows for higher sample throughput when used in conjunction with a highly efficient <2µm particle size column. The 1.9µm Pinnacle® DB Aqueous C18, in a 50 x 2.1mm configuration, is ideally suited for this application, as shown in Figure 2.

Using LC/MS/MS technology and Aqueous C18 columns, in combination with gas chromatography, results in the most comprehensive monitoring of pesticide residues. Labs interested in more complete multi-residue analysis of pesticides in food matrices, including difficult polar or thermally unstable compounds, should consider adding LC/MS/MS and Aqueous C18 columns to routine testing procedures. The Aqueous C18 phase is also available on 1.9µm Pinnacle® DB silica for UHPLC platforms.

Acknowledgements

The authors wish to thank the US FDA for their collaboration and recognize the participation of multiple FDA labs in this work.

Figure 1  More than 280 pesticide residues—including difficult polar species—show excellent peak shape and retention on a 3µm Ultra Aqueous C18 column.

A. Pesticides in positive ion mode.

PeakstR (min)Transition 1Transition 2
1.Acephate1.27184.1 -> 143184.1 -> 125
2.Acetamiprid4.44223.2 -> 126.1223.2 -> 99.1
3.Acibenzolar-S-methyl7.22211 -> 136211 -> 140
4.Alanycarb7.91400.1 -> 238.2400.1 -> 91.1
5.Aldicarb4.49208.2 -> 116.1208.2 -> 89.1
6.Aldicarb sulfone2.03223.1 -> 86.1223.1 -> 148
7.Aldicarb sulfoxide2.2207.1 -> 132.1207.1 -> 89.1
8.Ametryn6.96228.1 -> 186.1228.1 -> 96
9.Aminocarb5.37209.1 -> 137.1209.1 -> 152.1
10.Avermectin B1a11.2890.5 -> 305890.5 -> 145
11.Avermectin B1b11.4876.5 -> 291876.5 -> 145
12.Azoxystrobin6.78404.1 -> 372.1404.1 -> 344.1
13.Benalaxyl7.78326.2 -> 148.2326.2 -> 91.1
14.Bendiocarb5.1224.2 -> 109.2224.2 -> 167.2
15.Benfuracarb8.33411.2 -> 195.1411.2 -> 252.1
16.Benthiavalicarb6.87382.1 -> 116382.1 -> 180.1
17.Benthiavalicarb-isopropyl6.87382.1 -> 196.8382.1 -> 179.9
18.Benzoximate7.98364 -> 199364 -> 105
19.Bitertanol7.98338 -> 70338 -> 269
20.Boscalid6.98343 -> 307343 -> 140
21.Bromuconazole (isomer 1)7.36378 -> 159.1378 -> 161
22.Bromuconazole (isomer 2)8.05378.1 -> 159.1378.1 -> 161
23.Bufencarb5.18222.2 -> 95.1222.2 -> 71
24.Bupirimate7.65317 -> 166317 -> 108
25.Buprofezin8.53306.2 -> 201.1306.2 -> 116.2
26.Butafenacil7.08492.2 -> 331.1492.2 -> 180.1
27.Butocarboxim4.4191.1 -> 75191.1 -> 116
28.Butocarboximsulfoxid2.1207 -> 74.9207 -> 90
29.Butoxycarboxim1.95223.1 -> 106223.1 -> 166
30.Carbaryl5.63202.1 -> 145202.1 -> 127
31.Carbendazim4.52192.2 -> 160.2192.2 -> 132.1
32.Carbetamide4.74237 -> 192237 -> 118
33.Carbofuran5.18222.2 -> 123.1222.2 -> 165.2
34.Carboxine5.61236 -> 143236 -> 87
35.Carfentrazone ethyl7.53412 -> 346412 -> 366
36.Chlorfluazuron9.18540 -> 158540 -> 519.7
37.Chloroxuron7.53291 -> 72291 -> 218
38.Chlorpyrifos8.35350 -> 198350 -> 96.9
39.Chlorpyriphos-methyl7.88324 -> 125.1322 -> 125.1
40.Chlortoluron6.31213.1 -> 72.2213.1 -> 46.2
41.Cinidon-ethyl8.71394.1 -> 348.1394.1 -> 107
42.Clethodim5.81360 -> 164360 -> 268
43.Clofentezine8.27303 -> 138303 -> 102
44.Clomazone7.04240.1 -> 125240.1 -> 89.1
45.Clothianidin3.35250 -> 169.1250 -> 132
46.Cyanazine5.51241.2 -> 214.2241.2 -> 104.1
47.Cyazofamid7.4325 -> 108325 -> 261
48.Cycluron6.71199.1 -> 89.1199.1 -> 89
49.Cymoxanil3.91199 -> 128199 -> 111
50.Cyproconazole (isomer 1)7.45292.2 -> 70.2292.2 -> 125.2
51.Cyproconazole (isomer 2)7.44292.1 -> 70.2292.1 -> 125.2
52.Cyprodinil8.15226 -> 93226 -> 77
53.Cyromazine2.63167.2 -> 85.1167.2 -> 68.2
54.Demeton-S-methyl2.9230.9 -> 89.1230.9 -> 61
55.Demeton-S-methylsulfon5.6262.9 -> 108.9262.9 -> 169
56.Desethyl-atrazine3.9188.1 -> 146.2188.1 -> 104.1
57.Desisopropylatrazine3.2174.1 -> 104.1174.1 -> 96.1
58.Desmedipham6.23318 -> 182318 -> 136
59.Desmethylpirimicarb5.11225 -> 72225 -> 168.1
60.Diazinon7.88305.1 -> 169.2305.1 -> 97
61.Dichlorvos5.36221 -> 109.1223.1 -> 109.1
62.Diclobutrazol7.58328 -> 70328 -> 160
63.Dicrotophos3.47238 -> 112238 -> 193
64.Diethofencarb6.56268 -> 226268 -> 180
65.Difenoconazole (isomer 1)8.35406.2 -> 251.1408.2 -> 253.1
66.Difenoconazole (isomer 2)8.35406.1 -> 251.1408.1 -> 253.1
67.Difenoxuron6.78287.2 -> 123.2287.2 -> 72
68.Diflubenzuron7.62311 -> 158.2311 -> 141.2
69.Dimethenamide6.9276.2 -> 244.1276.2 -> 168.3
70.Dimethoate3.58230 -> 125230 -> 199.1
71.Dimethomorph7.22388.2 -> 301.1388.2 -> 165.2
72.Dimoxystrobin7.6327.1 -> 205327.1 -> 116
73.Diniconazol8.07326 -> 70326 -> 159
74.Dinotefuran2.02203.1 -> 114.1203.1 -> 129
75.Dioxacarb3.68224 -> 123224 -> 167.1
76.Diphenylamin7.03170.1 -> 93170.1 -> 92
77.Disulfoton6.08275.1 -> 89275.1 -> 61
78.Diuron6.7233.1 -> 72235.1 -> 72.1
79.Edifenphos6.66311 -> 283328 -> 283
80.EPN6.72324 -> 157.1324 -> 296
81.Epoxiconazole7.65330 -> 121330 -> 101
82.Etaconazole7.57328.2 -> 159.1328.2 -> 123
83.Ethiofencarb5.58226.1 -> 106.9226.1 -> 164.1
84.Ethiofencarbsulfoxid3.48242 -> 107242 -> 185.1
85.Ethion7.9385 -> 199385 -> 171
86.Ethiprole6.62397.3 -> 351397.3 -> 255.5
87.Ethofenprox9.66394.1 -> 107.1394.1 -> 177.2
88.Ethofumesate6.54304 -> 121304 -> 161
89.Ethoprophos5.98243 -> 131243 -> 97
90.Ethoxyquin7.4218.1 -> 174218.1 -> 160
91.Etoxazole9360.1 -> 141360.1 -> 57.2
92.Famoxadone7.72392 -> 331392 -> 238
93.Fenamidone6.65312.1 -> 92.1312.1 -> 65
94.Fenamiphos7.5304.2 -> 217.1304.2 -> 202.1
95.Fenarimol7.3331 -> 268331 -> 81
96.Fenazaquin9.91307 -> 161307 -> 147
97.Fenbuconazole7.57337 -> 125337 -> 70
98.Fenhexamid7.04302 -> 97302 -> 55
99.Fenitrothion6.4278 -> 125.2278 -> 109
100.Fenoxycarb7.53302.2 -> 88.1302.2 -> 116.2
101.Fenpropimorph9.84304 -> 147304 -> 117
102.fenpyroximate9.29422 -> 366.1442 -> 135.1
103.Fenthion6.9278.9 -> 169278.9 -> 246.9
104.Fenuron3.85165.1 -> 72.1165.1 -> 46
105.Flonicamid2.25230.1 -> 203.1230.1 -> 174
106.Flucarbazone2.81397.1 -> 130.1397.1 -> 115
107.Flufenacet7.17364.1 -> 152.2364.1 -> 194.2
108.Flufenoxuron8.98489.1 -> 158.2489.1 -> 141.2
109.Fluometuron5.98233.1 -> 72.1233.1 -> 46
110.Fluopicolide7.2385 -> 174.8383 -> 173
111.Fluoxastrobin7.34459.2 -> 427.2459.2 -> 188
112.Fluquinconazole7.31376 -> 349376 -> 307
113.Flusilazole7.6316 -> 247316 -> 165
114.Flutolanil6.81341.1 -> 242.1341.1 -> 262.1
115.Flutriafol5.99302 -> 123302 -> 109
116.Fonophos5.9247 -> 183247 -> 201
117.Forchlorfenuron6.37248 -> 93.1248 -> 165.1
118.Formetanate4.48222 -> 165.1222 -> 120
119.Fuberidazole5.5185 -> 157185 -> 65
120.Furalaxyl6.62302.1 -> 95.1302.1 -> 242.1
121.Furathiocarb8.42383.2 -> 195.2383.2 -> 252.2
122.Hexaconazole7.95314 -> 70314 -> 159
123.Hexaflumuron8.42461.1 -> 158.2461.1 -> 141.1
124.Hexythiazox8.77353 -> 228353 -> 168
125.Hydramethylnon9.2495.2 -> 323.1495.2 -> 151
126.Imazalil8.1297.1 -> 159.2299.1 -> 161.2
127.Imazapyr7.3262.2 -> 217.2262.2 -> 202.2
128.Imidacloprid3.82256.2 -> 209256.2 -> 175.2
129.Indoxacarb8.03528 -> 203528 -> 56
130.Ipconazole8.33334.2 -> 70334.2 -> 125
131.Iprodion7.6330.1 -> 244.9332.1 -> 247
132.Iprovalicarb6.98321.2 -> 119321.2 -> 203.2
133.Irgarol7.72254.2 -> 198.1254.2 -> 83.2
134.Isofenphos6.66314 -> 120314 -> 162.1
135.Isoprocarb5.87194.2 -> 95.1194.2 -> 137.2
136.Isoproturon6.42207.2 -> 72.1207.2 -> 46.1
137.Isoxaflutole5.87360.1 -> 251.1360.1 -> 220.1
138.Kresoxim-methyl7.53314 -> 116314 -> 206
139.Lenacil6.5235.3 -> 153.2235.3 -> 136.2
140.Linuron6.99249.1 -> 160249.1 -> 182.1
141.Lufenuron8.83511.1 -> 158.1511.1 -> 141.2
142.Malathion6.83331 -> 99.1331 -> 127.1
143.Mandipropamid6.81412.1 -> 328.1412.1 -> 355.9
144.Mefenacet7.35299 -> 148.1299 -> 120.1
145.Mepanipyrim7.57224 -> 106224 -> 77
146.Mepronil6.86270.1 -> 119.1270.1 -> 228
147.Metalaxyl6.13280.2 -> 220.2280.2 -> 192.3
148.Metconazole8.01320 -> 70320 -> 125
149.Methabenzthiazuron6.56222.1 -> 165.2222.1 -> 150.3
150.Methamidophos1.06142 -> 94142 -> 125
151.Methiocarb6.82226.1 -> 169.2226.1 -> 121.1
152.Methomyl2.62163.1 -> 88.1163.1 -> 106
153.Methoprotryne6.95272.2 -> 240.2272.2 -> 198
154.Methoxyfenozide6.9369 -> 149369 -> 133
155.Metobromuron6.22259 -> 170.2259 -> 148.2
156.Metolachlor7.5284.2 -> 252.2284.2 -> 176.2
157.Metoxuron5.1229 -> 72.1229 -> 156.1
158.Metribuzin5.14215.1 -> 187.2215.1 -> 84.1
159.Mevinphos4.29225 -> 127225 -> 193
160.Mexacarbate7.02223.2 -> 166.2223.2 -> 151
161.Milbemectin A310.3546.4 -> 511.3546.4 -> 493.3
162.Milbemectin A410.5560.4 -> 525.4560.4 -> 55.2
163.Molinate7.3188.2 -> 126.2188.2 -> 55.1
164.Monocrotophos2.9224 -> 127224 -> 98
165.Monolinuron5.93215.1 -> 126.1215.1 -> 99
166.Monuron5.7199.2 -> 72.2199.2 -> 126.3
167.Myclobutanil7.17289 -> 70289 -> 125
168.Neburon7.65275 -> 88275 -> 114
169.Nitenpyram2.55271.2 -> 126.1271.2 -> 237.2
170.Novaluron8.38493 -> 158.1493 -> 141.1
171.Nuarimol6.7315 -> 252315 -> 81
172.Omethoate1.69214 -> 124.9214 -> 182.8
173.Oxadixyl4.85279.2 -> 219.2279.2 -> 132.1
174.Oxamyl2.35237.1 -> 72.1237.1 -> 90.1
175.Oxydemeton-methyl3.1247 -> 169247 -> 109
176.Paclobutrazol6.82294 -> 70294 -> 125
177.Parathion-ethyl6.7292.1 -> 236.2292.1 -> 94.1
178.Parathion-methyl7.6263.9 -> 232.1263.9 -> 125
179.Penconazole8.01284 -> 159284 -> 70
180.Pencycuron8.1329.1 -> 125.1331.2 -> 127
181.Phenmedipham6.35301.1 -> 136301.1 -> 168.1
182.Phenthoate7321 -> 163321 -> 79
183.Phosmet6.7318 -> 160318 -> 133
184.Phoxim7.9299.1 -> 129.1299.1 -> 77.1
185.Picoxystrobin7.44368 -> 145368 -> 205
186.Pinoxaden7.99401.3 -> 317.2401.1 -> 57
187.Piperonyl butoxide8.62356.2 -> 177.2356.2 -> 119
188.Pirimicarb6.29239.2 -> 72.1239.2 -> 182.2
189.Pirimicarb- desmethylformamido6.4253.2 -> 72.1253.2 -> 225.3
190.Pirimiphos-ethyl7.48334 -> 198.1334 -> 182.1
191.Prochloraz8.29376.1 -> 308376.1 -> 70.1
192.Promecarb6.86208.2 -> 109.1208.2 -> 151.1
193.Prometon6.86226.1 -> 142.1226.1 -> 86
194.Prometryn7.4242.2 -> 200.1242.2 -> 158.1
195.Propachlor6.2212.2 -> 170.1212.2 -> 94.1
196.Propamocarb6.61189.2 -> 102.2189.2 -> 73.9
197.Propargite8.79368 -> 231368 -> 175
198.Propazine6.9230.1 -> 146.1230.1 -> 188.1
199.Propham5.78180 -> 138180 -> 120
200.Propiconazole7.98342.1 -> 159.1342.1 -> 69.1
201.Propoxur5.03210.1 -> 111210.1 -> 168.1
202.Prosulfocarb8.5252.3 -> 91.1252.3 -> 128.1
203.py Cinerin I9317.2 -> 149317.2 -> 106.9
204.py Cinerin II8.2361.2 -> 149361.2 -> 106.9
205.Pymetrozin3.61218 -> 105218 -> 78
206.Pyracarbolid5.4218.2 -> 125218.2 -> 97
207.Pyraclostrobin7.95388 -> 194388 -> 163
208.Pyrazophos7.8374 -> 222374 -> 194
209.Pyrethrin I8.9329.2 -> 160.9329.2 -> 132.9
210.Pyrethrin II8.3373.1 -> 160.9373.1 -> 308.9
211.Pyridaben9.33365 -> 147365 -> 309
212.Pyridaphenthion7.8341 -> 189341 -> 205
213.Pyrimethanil7.24200 -> 107200 -> 82
214.Pyriproxyfen8.72322 -> 96322 -> 185
215.Quinalphos6.7299 -> 147299 -> 163
216.Quinoxyfen9.12308 -> 197308 -> 162
217.Rotenone7.61395 -> 213395 -> 192
218.Secbumeton6.85226.2 -> 170.1226.2 -> 100
219.Siduron6.55233.3 -> 137.2233.3 -> 94
220.Simetryn6.36214 -> 124214 -> 144
221.Spinosyn A11.3732.6 -> 142.1732.6 -> 98
222.Spinosyn D11.6746.6 -> 142.1746.6 -> 98
223.Spirodiclofen8.96411.3 -> 313.2411.3 -> 213.1
224.Spiromesifen8.8371.3 -> 273371.3 -> 255
225.Spiroxamine (isomer 1)10.7; 11298.4 -> 144.2298.4 -> 100.2
226.Spiroxamine (isomer 2)10.7; 11298.3 -> 144.2298.3 -> 100.2
227.Sulfentrazone4.77387 -> 307.1387 -> 146
228.Sulfotep-ethyl7323 -> 115323 -> 171.1
229.Sulprofos7323 -> 219323 -> 247
230.Tebuconazole7.8308 -> 70308 -> 125
231.Tebufenozide7.39353.1 -> 133.1353.1 -> 297.1
232.Tebufenpyrad8.56334 -> 117334 -> 145
233.Tebuthiuron5.71229.2 -> 172.4229.2 -> 116.1
234.Teflubenzuron8.81381.1 -> 141.2381.1 -> 158.2
235.Terbufos6.5289 -> 103289 -> 57
236.Terbumeton6.84226 -> 170226 -> 114
237.Terbutryn7.57242.2 -> 186.1242.2 -> 68.1
238.Tetraconazole7.3372 -> 159372 -> 70
239.Thiabendazole5.71202.1 -> 175.1202.1 -> 131.2
240.Thiacloprid4.89253.1 -> 126.1253.1 -> 99.1
241.Thiamethoxam3.06292 -> 211292 -> 181
242.Thidiazuron5.18221.2 -> 102.1221.2 -> 127.9
243.Thiobencarb8.09258.1 -> 125258.1 -> 89
244.Thiofanox5.7219 -> 57.1219 -> 60.9
245.Thiofanoxsulfon3.4251.1 -> 75.9251.1 -> 57
246.Thiofanoxsulfoxid3.6235.1 -> 104.1235.1 -> 57
247.Thiophanate-methyl5.1343 -> 151343 -> 192
248.Tolclofos-methyl8301 -> 175301 -> 268.9
249.Topramezone1.73364.1 -> 334.1364.1 -> 125
250.Triadimefon6.94294 -> 197294 -> 225
251.Triadimenol7.04296.1 -> 70.1296.1 -> 227.2
252.Tricyclazole5.18190 -> 163190 -> 136
253.Trifloxystrobin8.09409 -> 186409 -> 206
254.Triflumizole8.47346 -> 278346 -> 73
255.Triflumuron7.94359.1 -> 156.2359.1 -> 139
256.Triticonazole7.38318 -> 70318 -> 125
257.Uniconazole7.4292.2 -> 70.1292.2 -> 43
258.Vamidothion3.75288 -> 146288 -> 118
259.Zoxamide7.7336.1 -> 186.9338.1 -> 188.7
Pesticides on Ultra Aqueous C18
LC_FF0490
ColumnUltra Aqueous C18 (cat.# 9178312)
Dimensions:100 mm x 2.1 mm ID
Particle Size:3 µm
Pore Size:100 Å
Temp.:35 °C
Samplemulticomponent pesticide standard
Diluent:water
Conc.:1 ppb each pesticide
Inj. Vol.:10 µL
Mobile Phase
A:10 mM NH4OAc in water
B:10 mM NH4OAc in methanol
Time (min)%B
0.0020
8.090
12.0100
14.8100
14.920
Flow:0.5 mL/min
DetectorApplied Biosystems/MDS Sciex LC/MS/MS
Model #:4000 QTRAP®
Ion Source:TurboIonSpray®
Ion Mode:ESI+
Ion Spray Voltage:5 kV
Gas 1:50 psi (344.7 kPa)
Gas 2:60 psi (413.7 kPa)
Source Temp.:600 °C
InstrumentShimadzu UFLCXR


B. Pesticides in negative ion mode.

PeakstR (min)Transition 1Transition 2
1.Acrinathrin9.09540 -> 372540 -> 299.9
2.Chlorfluazuron9.24539.9 -> 356.8539.9 -> 519.7
3.Clothianidin3.63249.9 -> 58247.9 -> 59
4.Diflubenzuron7.68309 -> 156.1310 -> 288.9
5.Diuron6.78230.9 -> 185.8230.9 -> 149.8
6.Fluazinam7.99462.5 -> 415.8462.5 -> 397.9
7.Fludioxonil6.93246.9 -> 179.9246.9 -> 125.9
8.Forchlorfenuron6.44246 -> 126.9246 -> 91.2
9.Hexaflumuron8.45459 -> 438.8459 -> 174.9
10.Imibenconazol8.82409 -> 250.9411 -> 253
11.Lufenuron8.87509 -> 325.9509 -> 175
12.Metaflumizon8.5505.1 -> 301.9505.1 -> 140.9
13.Metamitron3.97201 -> 184.8201 -> 116.9
14.Methoxyfenozid6.98366.9 -> 104.9366.9 -> 148.9
15.Nitenpyram2.59269.2 -> 221.6269.2 -> 100.8
16.Novaluron8.42491.1 -> 470.7493.1 -> 472.7
17.Profoxydim7.57464.3 -> 277.9464.3 -> 126.8
18.Propoxycarbazon3.09396.9 -> 156396.9 -> 112.9
19.Prothioconazol7.16342 -> 100.1343.9 -> 99.9
20.Tebufenozid7.46350.9 -> 149350.9 -> 105
21.Teflubenzuron8.85378.6 -> 338.8378.6 -> 195.9
22.Tepraloxydim4.57340 -> 248340 -> 220.1
23.Terbacil5.38214.9 -> 158.9216.9 -> 160.9
24.Tralkoxydim6.28328.1 -> 253.8328.1 -> 281.8
25.Triadimefon7.01292 -> 67.9292 -> 234.9
26.Triflumuron8356.9 -> 153.8358.9 -> 155.9
Pesticides on Ultra Aqueous C18
LC_FF0490A
ColumnUltra Aqueous C18 (cat.# 9178312)
Dimensions:100 mm x 2.1 mm ID
Particle Size:3 µm
Pore Size:100 Å
Temp.:35 °C
Samplemulticomponent pesticide standard
Diluent:water
Conc.:1 ppb each pesticide
Inj. Vol.:10 µL
Mobile Phase
A:10 mM NH4OAc in water
B:10 mM NH4OAc in methanol
Time (min)%B
0.0020
8.090
12.0100
14.8100
14.920
Flow:0.5 mL/min
DetectorApplied Biosystems/MDS Sciex LC/MS/MS
Model #:4000 QTRAP®
Ion Source:TurboIonSpray®
Ion Mode:ESI-
Ion Spray Voltage:-4.2 kV
Gas 1:50 psi (344.7 kPa)
Gas 2:60 psi (413.7 kPa)
Source Temp.:600 °C
InstrumentShimadzu UFLCXR


C. Improved retention of difficult pesticides.

PeakstR (min)Transition 1Transition 2
1.Methamidophos1.06142 -> 94142 -> 125
2. Acephate1.27184.1 -> 143184.1 -> 125
3.Omethoate1.69214 -> 124.9214 -> 182.8
4.Propamocarb6.61189.2 -> 102.2189.2 -> 73.9
Pesticides on Ultra Aqueous C18
LC_FF0490B
ColumnUltra Aqueous C18 (cat.# 9178312)
Dimensions:100 mm x 2.1 mm ID
Particle Size:3 µm
Pore Size:100 Å
Temp.:35 °C
Samplemulticomponent pesticide standard
Diluent:water
Conc.:1 ppb each pesticide
Inj. Vol.:10 µL
Mobile Phase
A:10 mM NH4OAc in water
B:10 mM NH4OAc in methanol
Time (min)%B
0.0020
8.090
12.0100
14.8100
14.920
Flow:0.5 mL/min
DetectorApplied Biosystems/MDS Sciex LC/MS/MS
Model #:4000 QTRAP®
Ion Source:TurboIonSpray®
Ion Mode:ESI+
Ion Spray Voltage:5 kV
Gas 1:50 psi (344.7 kPa)
Gas 2:60 psi (413.7 kPa)
Source Temp.:600 °C
InstrumentShimadzu UFLCXR

Figure 2  Higher sample throughput can be achieved using UHPLC and MS/MS with a 1.9µm Pinnacle® DB Aqueous C18 column.

PeakstR (min)PolarityMol. Wt. Transition 1
1.Methamidophos0.45positive141.13142.0→94.0
2.Acephate0.62positive183.17184.0→142.8
3.Bentazone0.77negative240.28239.0→131.8
4.Omethoate1.07positive213.14214.0→124.9
5.Bromoxynil1.32negative276.91275.9→80.8
6.Butoxycarboxin1.64positive222.27223.1→86.1
7.Aldicarb sulfoxide2.03positive206.26207.1→132.1
8.Methomyl2.08positive162.21163.1→88.1
9.Ioxynil2.46negative370.92369.8→126.7
10.Thiamethoxam2.7positive291.7292.0→211.0
11.Monocrotophos2.73positive223.17224.1→127.0
12.Dimethoate2.9positive229.26230.1→199.0
13.Fenuron3.1positive164.21165.1→72.1
14.Dioxacarb3.12positive223.23224.0→123.0
15.Dicrotophos3.28positive237.19238.0→112.0
16.Vamidothion3.45positive287.34288.0→146.0
17.Carbendazim3.73positive191.19192.0→160.0
18.Aldicarb3.73positive190.27208.1→116.0
19.Formetanate3.74positive221.26222.1→165.2
20.Acetamiprid3.95positive222.67223.1→126.1
21.Carbetamide3.99positive236.27237.0→192.0
22.Oxamyl3.99positive219.26237.1→72.2
23.Aminocarb4.11, 4.44positive208.26209.2→137.1
24.Propoxur4.15positive209.24210.1→111.0
25.Oxadixyl4.21positive278.31279.0→219.0
26.Bendiocarb4.24positive223.23224.1→109.1
27.Thiacloprid4.25positive252.71253.2→126.1
28.Thiophanate methyl4.3positive342.4343.0→151.0
29.Methabenzthiazuron4.31positive221.28222.0→165.1
30.Tricyclazole4.35positive189.23190.0→163.0
31.Pyracarbolid4.38positive217.27218.2→125.0
32.Propamocarb4.41positive188.27189.2→102.2
33.Carboxin4.51positive235.3236.0→143.0
34.Ethiofencarb4.52positive225.31226.1→106.9
35.Carbaryl4.58positive201.22202.1→145.1
36.Thiabendazole4.6positive201.25202.0→175.0
37.Carbanilide4.6positive212.25213.1→94.0
38.Clethodim4.61positive359.91360.0→164.0
39.Tebuthiuron4.68positive228.32229.2→172.4
40.Fluometuron4.75positive232.21233.1→72.0
41.Metobromuron4.82positive259.1259.0→170.2
42.Flutriafol4.84positive301.3302.0→123.0
43.Chlortoluron4.92positive212.68213.1→72.2
44.Simetryn4.96positive213.31214.0→124.0
45.Pirimicarb4.97positive238.29239.2→72.1
46.Forchlorfenuron5.04positive247.68248.0→129.1
47.Siduron5.09positive232.32233.3→137.2
48.Ethofumesate5.11positive286.35304.0→121.0
49.Cycluron5.13positive198.31199.1→89.1
50.Diuron5.13positive233.1233.1→72.0
51.Diethofencarb5.15positive267.33268.0→226.0
52.Furalaxyl5.18positive301.34302.2→95.0
53.Methiocarb5.24positive225.31226.1→169.2
54.Secbumeton5.24positive225.29226.2→169.9
55.Terbumeton5.25positive225.29226.2→169.9
56.Prometon5.26positive225.29226.2→142.3
57.Paclobutrazol5.26positive293.8294.0→70.0
58.Promecarb5.27positive207.27208.2→109.2
59.Dimoxystrobin5.27positive326.39327.1→205.0
60.Ametryn5.29positive227.33228.2→186.2
61.Methoprotryne5.32positive271.39272.2→240.2
62.Triadimefon5.32positive293.75294.0→197.0
63.Mexacarbate5.34positive222.28223.2→166.2
64.Fludioxonil5.34negative248.19247.0→179.9
65.Boscalid5.36negative343.21343.0→307.0
66.Azoxystrobin5.36positive403.3404.1→372.1
67.Methoxyfenozide5.38positive368.47369.0→149.0
68.Cyproconazole5.39positive291.78292.2→70.2
69.Prothioconazole5.41negative344.26341.9→305.8
70.Flufenacet5.46positive363.34364.0→152.0
71.Butafenacil5.47positive474.82492.2→331.1
72.Myclobutanil5.51positive288.78289.0→70.0
73.Dimethomorph5.52,5.54positive387.86388.0→301.0
74.Bromuconazole 475.54positive377.06378.0→159.0
75.Prometryn5.55positive241.36242.2→158.1
76.Fipronil5.56negative437.15434.9→329.8
77.Triticonazole5.58positive317.81318.0→70.0
78.Tetraconazole5.6positive372.12372.0→159.0
79.Uniconazole5.62positive291.78292.2→70.2
80.Fluoxastrobin5.62positive458.83459.2→427.2
81.Cyazofamid5.63positive324.78325.0→108.0
82.Terbutryn5.65positive241.36242.2→186.0
83.Tebufenozide5.65positive352.47353.1→133.1
84.Chloroxuron5.67positive290.75291.0→72.0
85.Picoxystrobin5.67positive367.25368.0→145.0
86.Carfentrazone ethyl5.69positive412.17412.0→346.0
87.Diclobutrazol5.71positive328.21328.0→70.0
88.Fenoxycarb5.72positive301.34302.0→88.1
89.Diflubenzuron5.72positive310.67311.2→158.1
90.Neburon5.74positive275.18275.0→88.0
91.Flusilazole5.76positive315.4316.0→247.0
92.Epoxiconazole5.76positive329.76330.0→121.0
93.Fenbuconazole5.76positive336.82337.0→125.0
94.Bupirimate5.77positive316.41317.0→166.0
95.Zoxamide5.77positive336.54336.2→187.1
96.Rotenone5.79positive394.42395.0→213.0
97.Benalaxyl5.83positive325.41326.0→148.0
98.Tebuconazole5.84positive307.82308.0→70.0
99.Penconazole5.93positive284.19284.0→159.0
100.Cyprodinil5.96positive225.29226.0→93.0
101.Propiconazole5.96positive342.22342.0→159.0
102.Alanycarb5.98positive399.52400.1→238.2
103.Triflumuron5.99positive358.68359.1→156.1
104.Thiobencarb6positive257.78258.1→125.0
105.Pyraclostrobin6positive387.83388.0→194.0
106.Benzoximate6.01positive363.8364.0→199.0
107.Pinoxaden6.01positive400.52401.3→317.2
108.Clofentezine6.11positive303.15303.0→138.0
109.Trifloxystrobin6.12positive408.38409.2→186.0
110.Prochloraz6.21positive376.67376.0→308.0
111.Difenoconazole6.29positive406.28406.0→251.0
112.Benfuracarb6.29positive410.53411.2→195.1
113.Triflumizole6.38positive345.75346.1→278.1
114.Buprofezin6.4positive305.44306.0→201.0
115.Piperonyl butoxide6.42positive338.45356.2→177.2
116.Pyriproxyfen6.52positive321.28322.0→96.0
117.Propargite6.68positive350.48368.0→231.0
118.Etoxazole6.87positive359.42360.1→141.0
119.Amitraz6.89positive293.41294.2→163.3
120.Noviflumuron7.08negative529.1527.1→343.8
121.Pyridaben7.18positive364.94365.0→147.0
122.Fenpyroximate7.2positive421.5422.0→366.0
123.Fenpropimorph7.38positive303.49304.0→147.0
124.Spiroxamine7.63,7.81positive297.48298.0→144.0
125.Spinosyn A8.37positive731.97732.6→142.2
Pesticides on Pinnacle DB Aqueous C18
LC_FF0479A
ColumnPinnacle® DB Aqueous C18 (cat.# 9418252)
Dimensions:50 mm x 2.1 mm ID
Particle Size:1.9 µm
Pore Size:140 Å
Temp.:35 °C
Samplemulticomponent pesticide standard
Diluent:water
Conc.:33.3 ppb each pesticide
Inj. Vol.:5 µL
Mobile Phase
A:10 mM NH4OAc in water
B:10 mM NH4OAc in methanol
Time (min)%B
0.0010
110
890
1090
1110
Flow:0.60 mL/min
Max Pressure:~517 bar
DetectorApplied Biosystems/MDS Sciex LC/MS/MS
Model #:4000 QTRAP® LC-MS/MS system
Ion Source:TurboIonSpray®
Ion Spray Voltage:5 kV
Gas 1:40 psi (275.8 kPa)
Gas 2:60 psi (413.7 kPa)
Source Temp.:500 °C
InstrumentShimadzu UFLCXR

Table 1  Peak list for pesticides in positive ion mode.

Compound ID Retention Time
(min)
Transition 1 Transition 2
Acephate1.27184.1 -> 143184.1 -> 143
Acetamiprid 4.44223.2 -> 126.1223.2 -> 99.1
Acibenzolar-S-methyl7.22211 -> 136211 -> 140
Alanycarb 7.91400.1 -> 238.2400.1 -> 91.1
Aldicarb4.49208.2 -> 116.1208.2 -> 89.1
Aldicarbsulfone2.03223.1 -> 86.1223.1 -> 148
Aldicarbsulfoxide 2.2207.1 -> 132.1207.1 -> 89.1
Ametryn6.96228.1 -> 186.1228.1 -> 96
Aminocarb5.37209.1 -> 137.1209.1 -> 152.1
Avermectin B1a11.2890.5 -> 305890.5 -> 145
Avermectin B1b 11.4876.5 -> 291876.5 -> 145
Azoxystrobin6.78404.1 -> 372.1404.1 -> 344.1
Benalaxyl7.78326.2 -> 148.2326.2 -> 91.1
Bendiocarb 5.1224.2 -> 109.2224.2 -> 167.2
Benfuracarb 8.33411.2 -> 195.1411.2 -> 252.1
Benthiavalicarb 6.87382.1 -> 116382.1 -> 180.1
Benthiavalicarb-isopropyl6.87382.1 -> 196.8382.1 -> 179.9
Benzoximate7.98364 -> 199364 -> 105
Bitertanol 7.98338 -> 70338 -> 269
Boscalid 6.98343 -> 307343 -> 140
Bromuconazole (isomer 1)7.36378 -> 159.1378 -> 161
Bromuconazole (isomer 2) 8.05378.1 -> 159.1378.1 -> 161
Bufencarb 5.18222.2 -> 95.1222.2 -> 71
Bupirimate 7.65317 -> 166317 -> 108
Buprofezin 8.53306.2 -> 201.1306.2 -> 116.2
Butafenacil7.08492.2 -> 331.1492.2 -> 180.1
Butocarboxim4.4191.1 -> 75191.1 -> 116
Butocarboximsulfoxid2.1207 -> 74.9207 -> 90
Butoxycarboxim 1.95223.1 -> 106223.1 -> 166
Carbaryl5.63202.1 -> 145202.1 -> 127
Carbendazim4.52192.2 -> 160.2192.2 -> 132.1
Carbetamide 4.74237 -> 192237 -> 118
Carbofuran 5.18222.2 -> 123.1222.2 -> 165.2
Carboxine 5.61236 -> 143236 -> 87
Carfentrazone-ethyl7.53412 -> 346412 -> 366
Chlorfluazuron9.18540 -> 158540 -> 383
Chloroxuron 7.53291 -> 72291 -> 218
Chlorpyrifos 8.35350 -> 198350 -> 96.9
Chlorpyrifos-methyl 7.88324 -> 125.1322 -> 125.1
Chlortoluron6.31213.1 -> 72.2213.1 -> 46.2
Cinidon-ethyl8.71394.1 -> 348.1394.1 -> 107
Clethodim 5.81360 -> 164360 -> 268
Clofentezine8.27303 -> 138303 -> 102
Clomazone7.04240.1 -> 125240.1 -> 89.1
Clothianidin 3.35250 -> 169.1250 -> 132
Cyanazine 5.51241.2 -> 214.2241.2 -> 104.1
Cyazofamid7.4325 -> 108325 -> 261
Cycluron 6.71199.1 -> 89.1199.1 -> 89
Cymoxanil 3.91199 -> 128199 -> 111
Cyproconazole (isomer 1)7.45292.2 -> 70.2292.2 -> 125.2
Cyproconazole (isomer 2)7.44292.1 -> 70.2292.1 -> 125.2
Cyprodinil8.15226 -> 93226 -> 77
Cyromazine2.63167.2 -> 85.1167.2 -> 68.2
Demeton-S-methyl2.9230.9 -> 89.1230.9 -> 61
Demeton-S-methyl-sulfon5.6262.9 -> 108.9262.9 -> 169
Desethyl-atrazine 3.9188.1 -> 146.2188.1 -> 104.1
Desisopropyl-atrazine3.2174.1 -> 104.1174.1 -> 96.1
Desmedipham 6.23318 -> 182318 -> 136
Desmethyl-pirimicarb 5.11225 -> 72225 -> 168.1
Diazinon 7.88305.1 -> 169.2305.1 -> 97
Dichlorvos5.36221 -> 109.1223.1 -> 109.1
Diclobutrazol7.58328 -> 70328 -> 160
Dicrotophos 3.47238 -> 112238 -> 193
Diethofencarb 6.56268 -> 226268 -> 180
Difenoconazole (isomer 1) 8.35406.2 -> 251.1408.2 -> 253.1
Difenoconazole (isomer 2)8.35406.1 -> 251.1408.1 -> 253.1
Difenoxuron6.78287.2 -> 123.2287.2 -> 72
Diflubenzuron 7.62311 -> 158.2311 -> 141.2
Dimethenamide6.9276.2 -> 244.1276.2 -> 168.3
Dimethoate 3.58230 -> 125230 -> 199.1
Dimethomorph 7.22388.2 -> 301.1388.2 -> 165.2
Dimoxystrobin 7.6327.1 -> 205327.1 -> 116
Diniconazole8.07326 -> 70326 -> 159
Dinotefuran 2.02203.1 -> 114.1203.1 -> 129
Dioxacarb 3.68224 -> 123224 -> 167.1
Diphenylamin7.03170.1 -> 93170.1 -> 92
Disulfoton 6.08275.1 -> 89275.1 -> 61
Diuron 6.7233.1 -> 72235.1 -> 72.1
Edifenphos6.66311 -> 283328 -> 283
EPN 6.72324 -> 157.1324 -> 296
Epoxiconazole7.65330 -> 121330 -> 101
Etaconazole7.57328.2 -> 159.1328.2 -> 123
Ethiofencarb5.58226.1 -> 106.9226.1 -> 164.1
Ethiofencarbsulfoxid 3.48242 -> 107242 -> 185.1
Ethion7.9385 -> 199385 -> 171
Ethiprole6.62397.3 -> 351397.3 -> 255.5
Ethofenprox 9.66394.1 -> 107.1394.1 -> 177.2
Ethofumesate 6.54304 -> 121304 -> 161
Ethoprophos 5.98243 -> 131243 -> 97
Ethoxyquin7.4218.1 -> 174218.1 -> 160
Etoxazole 9360.1 -> 141360.1 -> 57.2
Famoxadone7.72392 -> 331392 -> 238
Fenamidone6.65312.1 -> 92.1312.1 -> 65
Fenamiphos 7.5304.2 -> 217.1304.2 -> 202.1
Fenarimol 7.3331 -> 268331 -> 81
Fenazaquin9.91307 -> 161307 -> 147
Fenbuconazole 7.57337 -> 125337 -> 70
Fenhexamid7.04302 -> 97302 -> 55
Fenitrothion6.4278 -> 125.2278 -> 109
Fenoxycarb 7.53302.2 -> 88.1302.2 -> 116.2
Fenpropimorph9.84304 -> 147304 -> 117
Fenpyroximate9.29422 -> 366.1442 -> 135.1
Fenthion 6.9278.9 -> 169278.9 -> 246.9
Fenuron3.85165.1 -> 72.1165.1 -> 46
Flonicamid2.25230.1 -> 203.1230.1 -> 174
Flucarbazone 2.81397.1 -> 130.1397.1 -> 115
Flufenacet 7.17364.1 -> 152.2364.1 -> 194.2
Flufenoxuron 8.98489.1 -> 158.2489.1 -> 141.2
Fluometuron 5.98233.1 -> 72.1233.1 -> 46
Fluopicolid 7.2385 -> 174.8383 -> 173
Fluoxastrobin7.34459.2 -> 427.2459.2 -> 188
Fluquinconazole 7.31376 -> 349376 -> 307
Flusilazole7.6316 -> 247316 -> 165
Flutolanil 6.81341.1 -> 242.1341.1 -> 262.1
Flutriafol 5.99302 -> 123302 -> 109
Fonophos 5.9247 -> 183247 -> 201
Forchlorfenuron 6.37248 -> 93.1248 -> 165.1
Formetanate 4.48222 -> 165.1222 -> 120
Fuberidazole 5.5185 -> 157185 -> 65
Furalaxyl6.62302.1 -> 95.1302.1 -> 242.1
Furathiocarb8.42383.2 -> 195.2383.2 -> 252.2
Hexaconazole7.95314 -> 70314 -> 159
Hexaflumuron 8.42461.1 -> 158.2461.1 -> 141.1
Hexythiazox 8.77353 -> 228353 -> 168
Hydramethylnon9.2495.2 -> 323.1495.2 -> 151
Imazalil 8.1297.1 -> 159.2299.1 -> 161.2
Imazapyr7.3262.2 -> 217.2262.2 -> 202.2
Imidacloprid 3.82256.2 -> 209256.2 -> 175.2
Indoxacarb 8.03528 -> 203528 -> 56
Ipconazole 8.33334.2 -> 70334.2 -> 125
Iprodion7.6330.1 -> 244.9332.1 -> 247
Iprovalicarb 6.98321.2 -> 119321.2 -> 203.2
Irgarol 7.72254.2 -> 198.1254.2 -> 83.2
Isofenphos 6.66314 -> 120314 -> 162.1
Isoprocarb 5.87194.2 -> 95.1194.2 -> 137.2
Isoproturon 6.42207.2 -> 72.1207.2 -> 46.1
Isoxaflutole 5.87360.1 -> 251.1360.1 -> 220.1
Kresoxim-methyl 7.53314 -> 116314 -> 206
Lenacil 6.5235.3 -> 153.2235.3 -> 136.2
Linuron 6.99249.1 -> 160249.1 -> 182.1
Lufenuron 8.83511.1 -> 158.1511.1 -> 141.2
Malathion 6.83331 -> 99.1331 -> 127.1
Mandipropamid 6.81412.1 -> 328.1412.1 -> 355.9
Mefenacet 7.35299 -> 148.1299 -> 120.1
Mepanipyrim 7.57224 -> 106224 -> 77
Mepronil 6.86270.1 -> 119.1270.1 -> 228
Metalaxyl 6.13280.2 -> 220.2280.2 -> 192.3
Metconazole 8.01320 -> 70320 -> 125
Methabenzthiazuron 6.56222.1 -> 165.2222.1 -> 150.3
Methamidophos 1.06142 -> 94142 -> 125
Methiocarb 6.82226.1 -> 169.2226.1 -> 121.1
Methomyl 2.62163.1 -> 88.1163.1 -> 106
Methoprotryne 6.95272.2 -> 240.2272.2 -> 198
Methoxyfenozide6.9369 -> 149369 -> 133
Metobromuron 6.22259 -> 170.2259 -> 148.2
Metolachlor 7.5284.2 -> 252.2284.2 -> 176.2
Metoxuron 5.1229 -> 72.1229 -> 156.1
Metribuzin 5.14215.1 -> 187.2215.1 -> 84.1
Mevinphos 4.29225 -> 127225 -> 193
Mexacarbate7.02223.2 -> 166.2223.2 -> 151
Milbemectin A3 10.3546.4 -> 511.3546.4 -> 493.3
Milbemectin A4 10.5560.4 -> 525.4560.4 -> 55.2
Molinate7.3188.2 -> 126.2188.2 -> 55.1
Monocrotophos 2.9224 -> 127224 -> 98
Monolinuron 5.93215.1 -> 126.1215.1 -> 99
Monuron 5.7199.2 -> 72.2199.2 -> 126.3
Myclobutanil7.17289 -> 70289 -> 125
Neburon 7.65275 -> 88275 -> 114
Nitenpyram 2.55271.2 -> 126.1271.2 -> 237.2
Novaluron 8.38493 -> 158.1493 -> 141.1
Nuarimol 6.7315 -> 252315 -> 81
Omethoate 1.69214 -> 124.9214 -> 182.8
Oxadixyl 4.85279.2 -> 219.2279.2 -> 132.1
OxamyI 2.35237.1 -> 72.1237.1 -> 90.1
Oxydemeton-methyl 3.1247 -> 169247 -> 109
Paclobutrazol 6.82294 -> 70294 -> 125
Parathion-ethyl 6.7292.1 -> 236.2292.1 -> 94.1
Parathion-methyl 7.6263.9 -> 232.1263.9 -> 125
Penconazole 8.01284 -> 159284 -> 70
Pencycuron 8.1329.1 -> 125.1331.2 -> 127
Phenmedipham 6.35301.1 -> 136301.1 -> 168.1
Phenthoate 7321 -> 163321 -> 79
Phosmet 6.7318 -> 160318 -> 133
Phoxim 7.9299.1 -> 129.1299.1 -> 77.1
Picoxystrobin 7.44368 -> 145368 -> 205
Pinoxaden 7.99401.3 -> 317.2401.1 -> 57
Piperonyl butoxide 8.62356.2 -> 177.2356.2 -> 119
Pirimicarb 6.29239.2 -> 72.1239.2 -> 182.2
Pirimicarb-
  desmethylformamido
6.4253.2 -> 72.1253.2 -> 225.3
Pirimiphos-ethyl 7.48334 -> 198.1334 -> 182.1
Prochloraz 8.29376.1 -> 308376.1 -> 70.1
Promecarb 6.86208.2 -> 109.1208.2 -> 151.1
Prometon 6.86226.1 -> 142.1226.1 -> 86
Prometryn 7.4242.2 -> 200.1242.2 -> 158.1
Propachlor 6.2212.2 -> 170.1212.2 -> 94.1
Propamocarb 6.61189.2 -> 102.2189.2 -> 73.9
Propargite 8.79368 -> 231368 -> 175
Propazine 6.9230.1 -> 146.1230.1 -> 188.1
Propham 5.78180 -> 138180 -> 120
Propiconazole 7.98342.1 -> 159.1342.1 -> 69.1
Propoxur 5.03210.1 -> 111210.1 -> 168.1
Prosulfocarb 8.5252.3 -> 91.1252.3 -> 128.1
py Cinerin I 9317.2 -> 149317.2 -> 106.9
py Cinerin II 8.2361.2 -> 149361.2 -> 106.9
Pymetrozin 3.61218 -> 105218 -> 78
Pyracarbolid 5.4218.2 -> 125218.2 -> 97
Pyraclostrobin 7.95388 -> 194388 -> 163
Pyrazophos 7.8374 -> 222374 -> 194
Pyrethrin I 8.9329.2 -> 160.9329.2 -> 132.9
Pyrethrin II 8.3373.1 -> 160.9373.1 -> 308.9
Pyridaben 9.33365 -> 147365 -> 309
Pyridaphenthion7.8341 -> 189341 -> 205
Pyrimethanil 7.24200 -> 107200 -> 82
Pyriproxyfen8.72322 -> 96322 -> 185
Quinalphos 6.7299 -> 147299 -> 163
Quinoxyfen 9.12308 -> 197308 -> 162
Rotenone 7.61395 -> 213395 -> 192
Secbumeton 6.85226.2 -> 170.1226.2 -> 100
Siduron 6.55233.3 -> 137.2233.3 -> 94
Simetryn 6.36214 -> 124214 -> 144
Spinosyn A 11.3732.6 -> 142.1732.6 -> 98
Spinosyn D 11.6746.6 -> 142.1746.6 -> 98
Spirodiclofen 8.96411.3 -> 313.2411.3 -> 213.1
Spiromesifen 8.8371.3 -> 273371.3 -> 255
Spiroxamine (isomer 1) 10.7; 11298.4 -> 144.2298.4 -> 100.2
Spiroxamine (isomer 2) 10.7; 11298.3 -> 144.2298.3 -> 100.2
Sulfentrazone 4.77387 -> 307.1387 -> 146
Sulfotep-ethyl 7323 -> 115323 -> 171.1
Sulprofos 7323 -> 219323 -> 247
Tebuconazole 7.8308 -> 70308 -> 125
Tebufenozide 7.39353.1 -> 133.1353.1 -> 297.1
Tebufenpyrad 8.56334 -> 117334 -> 145
Tebuthiuron 5.71229.2 -> 172.4229.2 -> 116.1
Teflubenzuron 8.81381.1 -> 141.2381.1 -> 158.2
Terbufos 6.5289 -> 103289 -> 57
Terbumeton 6.84226 -> 170226 -> 114
Terbutryn 7.57242.2 -> 186.1242.2 -> 68.1
Tetraconazole 7.3372 -> 159372 -> 70
Thiabendazole 5.71202.1 -> 175.1202.1 -> 131.2
Thiacloprid 4.89253.1 -> 126.1253.1 -> 99.1
Thiamethoxam 3.06292 -> 211292 -> 181
Thidiazuron 5.18221.2 -> 102.1221.2 -> 127.9
Thiobencarb 8.09258.1 -> 125258.1 -> 89
Thiofanox 5.7219 -> 57.1219 -> 60.9
Thiofanoxsulfon3.4251.1 -> 75.9251.1 -> 57
Thiofanoxsulfoxid3.6235.1 -> 104.1235.1 -> 57
Thiophanate-methyl 5.1343 -> 151343 -> 192
Tolclofos-methyl 8301 -> 175301 -> 268.9
Topramezone 1.73364.1 -> 334.1364.1 -> 125
Triadimefon 6.94294 -> 197294 -> 225
Triadimenol 7.04296.1 -> 70.1296.1 -> 227.2
Tricyclazole 5.18190 -> 163190 -> 136
Trifloxystrobin 8.09409 -> 186409 -> 206
Triflumizole 8.47346 -> 278346 -> 73
Triflumuron 7.94359.1 -> 156.2359.1 -> 139
Triticonazole 7.38318 -> 70318 -> 125
Uniconazole 7.4292.2 -> 70.1292.2 -> 43
Vamidothion 3.75288 -> 146288 -> 118
Zoxamide 7.7336.1 -> 186.9338.1 -> 188.7

Data for 3µm Ultra Aqueous C18 column are shown.

Table 2  Peak list for pesticides in negative ion mode.

Compound ID Retention Time
(min)
Transition 1 Transition 2
Acrinathrin9.09540 -> 372540 -> 372
Chlorfluazuron9.24539.9 -> 356.8539.9 -> 356.8
Clothianidin3.63249.9 -> 58247.9 -> 59
Diflubenzuron 7.68309 -> 156.1310 -> 288.9
Diuron6.78230.9 -> 185.8230.9 -> 149.8
Fluazinam7.99462.5 -> 415.8462.5 -> 397.9
Fludioxonil6.93246.9 -> 179.9246.9 -> 125.9
Forchlorfenuron6.44246 -> 126.9246 -> 91.2
Hexaflumuron8.45459 -> 438.8459 -> 174.9
Imibenconazol8.82409 -> 250.9411 -> 253
Lufenuron8.87509 -> 325.9509 -> 175
Metaflumizon8.5505.1 -> 301.9505.1 -> 140.9
Metamitron3.97201 -> 184.8201 -> 116.9
Methoxyfenozid6.98366.9 -> 104.9366.9 -> 148.9
Nitenpyram2.59269.2 -> 221.6269.2 -> 100.8
Novaluron8.42491.1 -> 470.7493.1 -> 472.7
Profoxydim 7.57464.3 -> 277.9464.3 -> 126.8
Propoxycarbazon3.09396.9 -> 156396.9 -> 112.9
Prothioconazol 7.16342 -> 100.1343.9 -> 99.9
Tebufenozid7.46350.9 -> 149350.9 -> 105
Teflubenzuron8.85378.6 -> 338.8378.6 -> 195.9
Tepraloxydim4.57340 -> 248340 -> 220.1
Terbacil5.38214.9 -> 158.9216.9 -> 160.9
Tralkoxydim6.28328.1 -> 253.8328.1 -> 281.8
Triadimefon7.01292 -> 67.9292 -> 234.9
Triflumuron8356.9 -> 153.8358.9 -> 155.9

Data for 3µm Ultra Aqueous C18 column are shown.

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