228 / 302
10
PAH
MDL
(ng/L)
RL
(ng/L)
Measured
Conc
(ng/L)
Measured
Conc
(ng/L)
Measured
Conc
in Fortified
Matrix
Experiment
(ng/L)
Fortification
Level
(ng/L)
% Recovery
Acenaphthene
15
45
-
-
203
176
115
Acenaphthylene
16
49
-
-
162
176
92
Antracene
29
86
-
-
185
176
105
Benz[
a
]anthracene
12
36
-
-
164
176
117
Benzo[
b
]
fluoranthene,
perylene
34
102
-
-
363
373
97
Benzo[
g,h,i
]
perylene
19
57
-
-
150
176
85
Benzo[
k
]
fluoranthene
21
63
-
-
219
176
124
Crysene
11
33
-
-
210
176
119
Dibenz[
a,h
]
anthracene
16
48
-
-
156
176
88
Fluoranthene
12
36
-
-
209
176
116
Fluorene
7.9
24
-
-
168
176
95
Indeno[1,2,3-
cd
]
pyrene
26
78
-
-
174
176
99
Naphthalene
20
60
-
-
161
176
91
C1-naphthalenes
13
40
-
-
364
353
103
C2-naphthalenes
15
44
-
<RL
228
176
118
Phenanathrene
19
57
-
-
175
176
99
Pyrene
17
50
-
-
200
176
111
Total PAH
0
0
% Recovery
Average
104±12
Table 4. Method performance upon analysis of reclaimed water obtained from the Miami-Dade North District Wastewater Treatment
Plant for US EPA priority PAHs.
Conclusion
An automated protocol for the comprehensive analysis of
28 parent PAHs and their extended alkylated homologues
by online SPE-LC-MS/MS was successfully developed
with optimized parameters for extraction, separation, and
detection using dopant-assisted APPI. Method
performance and the control of matrix effects were
demonstrated by obtaining good recoveries upon analysis
of seawater, reclaimed water, and rainwater runoff fortified
with certified standards, showing the utility of this method
to survey the occurrence of PAHs in waters at the urban
environment. A survey of PAH concentration in a seawater
environment influenced by a large urban area was
conducted, and although background concentrations were
below MDLs, localized PAH input events from boating
activities were detected above reporting limits. With lower
run times, very simple sample preparation, lower
generation of toxic solvent waste, and higher sensitivity
per volume of sample used, this method could represent a
viable alternative to LLE-GC-MS for routine PAH
monitoring, providing laboratories with a much higher
sample throughput while reducing overall operation costs
and the environmental impact of PAH analysis.