72
Table 16: Comparison of quantification of chlordanes [ng/g dw] in sediments by ECNI (two instruments)
and EI-MS/MS. The fraction of the Florisil clean-up is assigned, where the compound is present.
Sample
Method
Hepta-
tram-
cis-
tram-
cis-
chlor
Chlordane
Chlordane
Nonachlor
Nonachlor
Florisil fraction
FI
F2
F2
F1+F2
F2
721 (2004)
EI-MS/MS
0.054
0.153
0.116
0.13
0.039
ECNI, 1200L
0.061
0.142
0.141
0.10
0.034
ECNI, HP 5989B
0.064
0.135
0.126
0.10
0.029
Average ± STD
0.056±
0.143±
0.128±
0.110±
0.034±
0.005
0.007
0.010
0.014
0.004
ODER (2004)
EI-MS/MS
0.056
0.066
0.083
0.12
0.021
ECNI, 1200L
0.036
0.078
0.044
0.10
0.026
ECNI, HP 5989B
0.042
0.059
0.060
0.09
0.017
Average ± STD
0.045±
0.068±
0.062±
0.103±
0.021±
0.008
0.008
0.016
0.012
0.004
715 (2004)
EI-MS/MS
<0.4
0.047
0.027
0.60
0.023
ECNI, 1200L
<1.3
0.049
0.038
0.50
0.024
ECNI, HP 5989B
<1.6
0.042
0.031
0.50
0.021
Average ± STD
0.046±
0.032±
0.53±
0.023±
0.003
0.005
0.05
0.001
RÜDEN
EI-MS/MS
<0.4
0.018
0.023
0.20
0.011
(2004)
ECNI, 1200L
<1.3
0.014
0.025
0.16
0.013
ECNI, HP 5989B
<1.6
0.006
0.016
0.15
0.006
Average ± STD
0.013±
0.021±
0.17±
0.010±
0.005
0.004
0.02
0.003
ECKFBU
EI-MS/MS
<0.4
0.047
0.033
0.17
0.032
(2004)
ECNI, 1200L
<1.3
0.044
0.054
0.15
0.027
ECNI, HP 5989B
<1.6
0.036
0.035
0.14
0.019
Average ± STD
0.042±
0.041±
0.15±
0.026±
0.005
0.009
0.01
0.005
STD: Standard deviation
5.3.7 Method validation and quality control
5.3.7.1 Limits of detection and quantification
Typically, limits of detection (LOD, signal-to-noise ratio 3:1) for s- or mPCAs in fish
liver were about 1 ng/g and limits of quantification (LOQ, signal-to-noise ratio 10:1)
were ca. 3 ng/g. Chlordanes could be identified down to 1-3 pg/g and quantified from
ca. 2-10 pg/g and onwards.
Single PCA congener groups in sediments were detectable down to ca. 5-50 ng/g
depending on their structure. Limits of quantification were about 3-5 times higher.
Total PCAs in sediments could be quantified with EI-MS/MS down to 2-8 ng/g.
