Contenu connexe Similaire à Chemistry Matters Dioxin2016 Analytical Summary (20) Plus de Chemistry Matters Inc. (20) Chemistry Matters Dioxin2016 Analytical Summary7. © 2016
Chemistry Ma2ers Inc.
• Chromatogram of early dioxin
analysis of Agent Orange
• Inves@gators began by
iden@fying all congeners for
chlorinated dioxins and furans in
the chromatograms
– 210 congeners exist
• Using mass spectrometry and
glass packed columns
• Synthesized compounds for
posi@ve iden@fica@on
7
Rappe C et al., Chemosphere, 1978, 5, 431–438.
Dioxin 2016 – Florence, Italy
Rappe C, Gara A, Buser H.R, Chemosphere, 1978, 12, 981 – 991.
Early Inves=ga=ons in Dioxin Contamina=on
in Agent Orange and Chlorinated Phenols
16. © 2016
Chemistry Ma2ers Inc.
Interlaboratory Studies
16
Histogram
2,3,4,7,8-PeCDF
Sugar Beat Pulp Results - 2,3,4,7,8-PeCDF
Reported results: 87
Report results > LOQ: 86
Robust mean: 0.88 ng/kg (CV: 30%)
Median: 0.89 ng/kg
Modes: 0.81 ng/kg, 1.03 ng/kg
Contribution to WHO-PCDD/F-TEQ: ca. 50 %
Dioxin 2016 – Florence, Italy
17. © 2016
Chemistry Ma2ers Inc.
c:Xcalibur...cdx_240315cdx_240315-16 3/25/2015 1:34:24 AM Zuckerrübenschnitzel-sugar beet pulp_t
150141982-001
RT: 19.31 - 21.21
19.4 19.5 19.6 19.7 19.8 19.9 20.0 20.1 20.2 20.3 20.4 20.5 20.6 20.7 20.8 20.9 21.0 21.1 21.2
Time (min)
0
20
40
60
80
100
0
20
40
60
80
100
0
20
40
60
80
100
RelativeAbundance
0
20
40
60
80
100
RT: 19.46
AA: 727412
RT: 20.94
AA: 584377
RT: 19.52
AA: 580258 RT: 20.44
AA: 389185
RT: 19.94
AA: 256338 RT: 21.01
AA: 251896RT: 20.26
AA: 169059
RT: 20.03
AA: 182541 RT: 20.12
AA: 90417
RT: 19.82
AA: 83916
RT: 19.66
AA: 53010
RT: 20.59
AA: 31000
RT: 19.46
AA: 455035 RT: 20.93
AA: 360979
RT: 19.52
AA: 352698 RT: 20.44
AA: 238310
RT: 19.93
AA: 161784 RT: 21.01
AA: 155133RT: 20.26
AA: 106435
RT: 20.03
AA: 106185 RT: 20.11
AA: 57517
RT: 19.82
AA: 50238
RT: 19.66
AA: 31708
RT: 20.59
AA: 18870 RT: 21.15
AA: 755
RT: 21.01
AA: 181912
RT: 20.25
AA: 53012
RT: 20.44
AA: 1830
RT: 20.93
AA: 862
RT: 21.15
AA: 441
RT: 19.93
AA: 340
RT: 19.52
AA: 422
RT: 19.39
AA: 284
RT: 21.01
AA: 113616
RT: 20.24
AA: 30769
RT: 20.46
AA: 431
RT: 20.88
AA: 507
RT: 20.41
AA: 276
RT: 20.59
AA: 283
RT: 20.01
AA: 252
RT: 19.95
AA: 170
RT: 19.47
AA: 98.68
NL:
1.77E5
m/z=
339.8595-
339.8601
MS ICIS
cdx_24031
5-16
NL:
1.09E5
m/z=
341.8566-
341.8572
MS ICIS
cdx_24031
5-16
NL:
5.86E4
m/z=
351.8996-
351.9004
MS ICIS
cdx_24031
5-16
NL:
3.33E4
m/z=
353.8966-
353.8974
MS ICIS
cdx_24031
5-16
It S=ll Comes Down to Chromatography
2,3,4,7,8-PeCDF
DB-5 MS (Agilent)
c:Xcalibur...cdx_200215cdx_200215-31 3/4/2015 8:28:08 PM 1 Animal Feed 1501-AFB-74.1_t
AFB-74.1
RT: 26.77 - 34.51
40
60
80
100
0
20
40
60
80
100
0
20
40
60
80
100
RelativeAbundance
0
20
40
60
80
100
RT: 28.17
AA: 28645 RT: 33.31
AA: 28793RT: 27.44
AA: 33942 RT: 28.66
AA: 24124
RT: 30.64
AA: 16621
RT: 27.75
AA: 13713 RT: 30.59
AA: 6037
RT: 27.22
AA: 6541 RT: 30.00
AA: 4640
RT: 31.59
AA: 3998
RT: 33.74
AA: 3370
RT: 31.19
AA: 2599
RT: 33.53
AA: 441
RT: 28.17
AA: 18462 RT: 33.31
AA: 18170RT: 27.45
AA: 21557
RT: 28.66
AA: 15302
RT: 30.64
AA: 10406
RT: 27.75
AA: 8864
RT: 30.59
AA: 3999
RT: 27.23
AA: 4251
RT: 30.00
AA: 2758
RT: 31.59
AA: 2671
RT: 33.75
AA: 1359
RT: 31.19
AA: 1785
RT: 33.55
AA: 250
RT: 30.74
AA: 164
RT: 33.29
AA: 34396
RT: 27.41
AA: 7541
RT: 28.02
AA: 287
RT: 33.40
AA: 124
RT: 32.78
AA: 124
RT: 28.65
AA: 237
RT: 32.99
AA: 105
RT: 33.27
AA: 21044
RT: 27.42
NL:
5.58E3
m/z=
339.8595-
339.8601
MS ICIS
cdx_20021
5-31
NL:
3.69E3
m/z=
341.8566-
341.8572
MS ICIS
cdx_20021
5-31
NL:
6.28E3
m/z=
351.8996-
351.9004
MS ICIS
cdx_20021
5-31
NL:
3.57E3
m/z=
353.8966-
353.8974
MS ICIS
cdx_20021
5-31
Rtx-2330 (Restek)
• Values from ‘expert’ labs similar to other labs, therefore
even experienced labs were not getting the identification
correct.
• Analysts need to know their chromatograms.
• High TEQ, makes this compound important for studies.
2,3,4,7,8-PeCDF
Dioxin 2016 – Florence, Italy 17
22. © 2016
Chemistry Ma2ers Inc.
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