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LC Technical Note
Simultaneous analysis of tap water pesticides
by LC/MS/MS
135
GL Sciences Inc.
Testing methods of Japanese Water Supply Act were revised in April 2013, and 64 pesticides were added to the target
compounds of the simultaneous analytical method using LC/MS/MS. In this note, an InertSustain C18 HPLC column
and a 4000QTRAP® linear tandem mass spectrometer (AB Sciex) were used. As a result, all the compounds added by
the revision were detected with excellent peak shape.
Intensity, cps
3.0e5
2.8e5
2.6e5
2.4e5
2.2e5
2.0e5
1.8e5
1.6e5
1.4e5
1.2e5
1.0e5
8.0e4
6.0e4
4.0e4
2.0e4
0.0
Positive
5
10
15
20
25
30
Time, min
35
40
45
50
1.00e5
55
Negative
9.00e4
8.00e4
7.00e4
Intensity, cps
6.00e4
5.00e4
4.00e4
3.00e4
2.00e4
1.00e4
0.00
5
10
Compound n ame
M.W.
Di notefura n
202.2
270.7
219.3
217.2
291.7
223.2
255.7
249.7
252.3
413.4
222.7
252.7
414.4
1
240.7
398.4
214.3
261.1
223.2
327.3
333.8
284.3
249.1
361.4
227.3
210.3
343.2
291 8
291.8
361.4
291.8
302.8
447.0
255.1
241.4
293.4
394.5
372.1
340.8
291.4
352.5
366.0
307.8
225.3
Ni tenpyra m
Oxa myl
Pymetrozi ne
Thi amethoxa m
Monocrotophos
Imi da cl ipri d
Cl othi ani din
Trinexa pa c‐ethyl
Ci nos ul furon
Acetami pri d
Thi aclopri d
Pyra zos ulfuron‐ethyl
Cya na zi ne
Ethoxys ulfuron
Metri buzi n
Broma ci l
Bendi ocarb
Fl uazifop
Furametpyr
Metominos trobin(E)
Li nuron
Pyri minobac‐methyl(Z)
Ametryn
Aci benzol a r‐s ‐methyl
Bos ca li d
Cyprocona zol e
Pyri minobac‐methyl(E)
Cyprocona zol e
Cumyl uron
Benzobi cycl on
Di clomezi ne
Prometryn
Si mecona zol e
Chroma fenozi de
Tetra cona zole
Inda nofa n
Na proa nil i de
Tebucona zol e
Tetra chl orvinphos (CVMP)
Di fl ubenzuron
Cyprodi nil
RT
(min)
6.1
6.7
6.7
7.2
7.3
7.6
8.2
8.3
8.5
8.6
9.0
10.1
11 1
11.1
13.2
14.1
14.1
14.1
15.0
17.1
19.5
22.7
24.8
24.9
25.2
25.3
26.5
27 3
27.3
28.4
28.8
29.2
29.3
29.7
30.4
30.7
30.9
31.4
32.3
33.3
33.5
33.6
34.0
35.6
15
Ionization
ESI (+)
ESI (+)
ESI (+)
ESI (+)
ESI (+)
ESI (+)
ESI (+)
ESI (+)
ESI (+)
ESI (+)
ESI (+)
ESI (+)
ESI
S (+)
( )
ESI (+)
ESI (+)
ESI (+)
ESI (+)
ESI (+)
ESI (+)
ESI (+)
ESI (+)
ESI (+)
ESI (+)
ESI (+)
ESI (+)
ESI (+)
ESI (+)
ESI (+)
ESI (+)
ESI (+)
ESI (+)
ESI (+)
ESI (+)
ESI (+)
ESI (+)
ESI (+)
ESI (+)
ESI (+)
ESI (+)
ESI (+)
ESI (+)
ESI (+)
20
Monitoring ion (m/z)
Prec ursor
Product
203
129
87
271
126
237
237
72
90
218
105
78
292
211
181
224
127
193
256
209
175
250
169
132
253
69
207
414
183
83
223
126
90
253
126
90
415
1
182
83
241
214
104
399
261
218
215
187
49
261
205
188
224
167
109
328
282
254
334
157
290
285
194
140
249
182
160
362
330
284
228
186
96
211
136
211
343
307
140
292
70
125
362
330
284
292
70
125
303
185
125
447
257
229
255
89
159
242
158
200
294
70
73
395
175
147
372
159
70
341
175
187
292
171
120
353
133
297
367
127
206
308
70
125
226
93
77
More technical information is here ・・・
25
30
Time, min
35
40
Compound name
M.W.
Etobenza ni de
340.2
341.2
406.3
439.3
406.3
305.3
298.3
345.8
431.3
372.8
376.3
324.2
353 8
353.8
293.4
408.6
Oxa di a rgyl
Di fenoconazole
Pyra zol ate
Di fenoconazole
Pi ri mi phos ‐methyl
Phoxi m
Trifl umi zol e
Benzofena p
Qui za l ofop‐ethyl
Oxa zi cl omefone
Cl omeprop
Pentoxa zone
Ami traz
Si la fl uofen
Compounbd name
M.W.
MCPA
200.6
235.1
218.1
338.8
267.7
415.2
310.7
528.1
465.1
Di chl orprop
Propa nil
Ina benfi de
Ti adi nil
Fentra za mi de
Di fl ubenzuron
Thifl uza mi de
Fl ua zina m
RT
(min)
36.2
38.0
38.5
38.7
38.8
39.2
39.3
40.7
41.5
42.1
42.4
42.7
43 0
43.0
46.1
48.0
RT
(min)
11.5
14.4
24.5
25.3
27.8
31.7
32.8
33.0
42.5
45
Ionization
ESI (+)
ESI (+)
ESI (+)
ESI (+)
ESI (+)
ESI (+)
ESI (+)
ESI (+)
ESI (+)
ESI (+)
ESI (+)
ESI (+)
ESI (+)
( )
ESI (+)
ESI (+)
Ionization
ESI (-)
ESI (-)
ESI (-)
ESI (-)
ESI (-)
ESI (-)
ESI (-)
ESI (-)
ESI ((-))
50
55
Monitoring ion (m/z)
Pre cursor
Product
340
179
149
358/223
341
223
406
251
337
439
91
173
406
251
337
306
164
108
299
77
129
346
278
73
431
105
119
373
299
271
376
190
161
324
120
203
354
286
186
294
163
122
426
287
168
Monitoring ion (m/z)
Product
Precursor
199
141
233
161
125
216
160
35
337
122
78
266
71
238
413
171
179
309
156
289
527
125
166
463
416
398
(1.0 g/L each)
HPLC Conditions;
: InertSustain C18 (3 m, 75 x 2.1 mm I.D.)
: A) 5 mM ammonium acetate in water
: B) 5 mM ammonium acetate in methanol
: A/B = 95/5 －4 min － 60/40 －35 min － 25/75
－5 min － 0/100 – 6 min – 0/100 –
－（equilibration
q
for 10 min）, v/v
Flow rate
: 0.15 mL/min
Col. Temp. : 40 ℃
Sample Temp.: 5 ℃
Detection
: MS/MS (4000 QTRAP®: ESI, MRM)
Inj. Volume : 100 L
Column
Eluent
http://www.glsciences.com/applications.html
GL Sciences LC Technical Note
＜Compounds detected in positive mode (1)＞
Cyproconazole and difenoconazole are detected as two peaks owing to existence of their isomers.
Acibenzolar
ib
l
-s-methyl
Ametryn
Benzofenap
Boscalid
Bromacil
Chromafenozide
Clothianidin
Cumyluron
Cyanazine
Cyproconazole 1
Q1/Q3=292/70
Diclomezine
Difenoconazole
Dinotefuran
Ethoxysulfuron
Fluazifop
Furametpyr
Acetamiprid
Imidacliprid
Amitraz
Indanofan
Bendiocarb
Cinosulfuron
Cyproconazole 2
Q1/Q3=292/125
Etobenzanide
Benzobicyclon
Clomeprop
Cyprodinil
Fentrazamide
GL Sciences LC Technical Note
＜ Compounds detected in positive mode (2) ＞
Linuron
Metominostrobin(E)
Oxadiargyl
Prometryn
Quizalofop-ethyl
Tetraconazole
Oxamyl
Pymetrozine
Silafluofen
Thiacloprid
Metribuzin
Oxaziclomefone
Monocrotophos
Naproanilide
Pentoxazone
Phoxim
Pyrazolate
Pyrazosulfuron-ethyl
Simeconazole
Tebuconazole
Tebufenozide
Thiamethoxam
Triflumizole
Trinexapac-ethyl
Nitenpyram
Pirimiphos-methyl
Pyriminobac-methyl(E) Pyriminobac-methyl(Z)
Tetrachlorvinphos
(CVMP)
GL Sciences LC Technical Note
＜ Compounds detected in negative mode ＞
Dichlorprop
Propanil
Diflubenzuron
Thifluzamide
Flusulfamide
Fluazinam
Inabenfide
MCPA
Tiadinil
HPLC column
Instruments
InertSustain C18 3 m, 75 x 2.1 mm I.D.
Cat.No. 5020-07413
LC800
C t t us
Contact
GL Sciences, Inc. Japan
22-1 Nishishinjuku 6-chome, Shinjuku-ku, Tokyo, 163-1130 Japan
TEL: +81-3 (5323)6620 FAX: +81-3 (5323)6621
GL Sciences,
Sciences Inc.
Inc USA
4733 Torrance Blvd. Ste 255, Torrance, CA 90503
Tel: (310)265-4424 FAX (310)265-4425
Distributors Outside of Japan and USA
GL Sciences uses distributors in many countries.
You can find a local distributor in your country in the
following url.
http://www.glsciences.com/distributors/
E-MAIL: world@gls.co.jp
4000 QTRAP®
（AB SCIEX）