17 / 71
M
astovska
et al
.:
J
ournal of
AOAC I
nternational
V
ol
.
98, N
o
. 2, 2015
491
maintenance to ensure adequate operation of the GC instrument.
Perform system checks.
(
b
)
MS conditions.
—Any GC/MS instrument (single
quadrupole, triple quadrupole, TOF, or ion trap) with EI may
be used as long as it provides results meeting the laboratory
qualification requirements. The 10 study participants used
the following instruments: single quadrupole (Agilent 5973–
Laboratory 4; Agilent 5975B XL Inert–Laboratories 3 and
8–10; Agilent 5975C–Laboratories 6 and 7), triple quadrupole
(Agilent 7000B–Laboratory 5; Thermo TSQ–Laboratory 1),
and time-of-flight (Leco Pegasus 4D–Laboratory 2). Pay special
attention to the optimization of the MS transfer line and MS
source temperature. Higher MS source temperatures are
recommended (e.g., ≥280°C for Agilent sources) to provide
optimum analysis (quantitative transfers, minimum peak
tailing) for less volatile PAHs.
Table
2014.08H
provides MS ions (
m/z
) and MS/MS
transitions used by the study participants for quantification and
identification of target PAHs and
13
C-PAHs using single-stage
MS (single quadrupole and TOF) and tandem MS/MS (triple
quadrupole) instruments, respectively.
Use adequate data acquisition rate (dwell times in scanning
instruments) and solvent delay time. Perform air/water
checks and autotune to verify and obtain adequate operation
Table 2014.08H. MS ions (
m
/
z
) and MS/MS precursor to product ion transitions used by study participants for
quantification (quant) and identification (qual) of target PAHs and
13
C-PAHs using single-stage MS (single quadrupole and
TOF) and tandem MS/MS (triple quadrupole) instruments, respectively
Single quad/TOF MS
Triple quad MS/MS
Compound
Quant
Qual
Quant
Qual
1,7-DMP
206
191
206>190
206>205, 206>165
1-MN
142
115
142>115
142>141, 142>116
1-MP
192
189
192>191
192>165
2,6-DMN
156
141, 144
156>115
156>141
3-MC
242
241
242>239
242>226
Ant
178
177
178>176
178>177, 178>151
BaA
228
226
228>226
228>224, 228>202
BaP
252
253
252>250
250>248, 252>224
BbF
252
253
252>250
250>248, 252>224
BghiP
276
277
276>274
274>272, 276>275
BkF
252
253
252>250
250>248, 252>224
Chr
228
226
228>226
228>224, 228>202
DBahA
278
276
278>276
276>274, 278>274
Fln
166
165
166>165
166>164, 166>163
Flt
202
200
202>200
202>201
IcdP
276
277
276>274
274>272, 276>248
Naph
128
127
128>102
128>127
Phe
178
177
178>176
178>177, 178>151
Pyr
202
200
202>200
202>201
13C-Ant
184
183
184>183
184>182, 184>156
13C-BaA
234
232
234>232
234>206
13C-BaP
256
257
256>254
256>228
13C-BbF
258
259
258>256
258>255
13C-BghiP
288
289
288>286
288>287
13C-BkF
258
259
258>256
258>255
13C-Chr
234
232
234>232
234>206
13C-DBahA
284
282
284>282
284>280
13C-Fln
172
171
172>171
172>170
13C-Flt
208
205
208>206
208>207
13C-IcdP
282
283
282>280
282>281
13C-Naph
134
133
134>133
134>105
13C-Phe
184
183
184>183
184>156
13C-Pyr
205
203, 206, 208
205>203
205>204