Document KR1KrdroVDna8k095epL3BOkw
AR226-3347
Analytical challenges in determination of Telo Alcohol and Telomer-derived fluorosurfactan polymers4n biological and environmental ma
Bogdan Szostek^^lteith B. Prickett1, S. Mark Kenne and Mary A. Kaiser2
lDuPont Haskell Laborato^ foHiealth and Environme
Sciences^fewarky^DE, USA
2 DuPont Centra I Research andDwe/opment^Wfmington
USA
SETAC Europe 13th Annual Meeting, Hamburg, Germany
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Basics of GEMS method -- EI spectra
}
[my] peldsnqmil]
MTBE
Ethyl Acetate
MeOH IPA
method - Chromatography
Column perfor
Abundance
7000
6000
5000
4000
3000
2000
< / 1000
Time->
3. i0 3.80 4.00 4.20 4.40 4.60 4.80 5.00 5.20 5.4
Ahis^-iAnM
7000 6000 5000
9
00 N)
I--1
>
4000
| 3000
i 2000
L 1000
'Jl-Y~^- time-,
3.60 3.80 4.00 4.20 4.40 4.60 4.80 5.00 5.20 5.
Abndantf"
7000
6000 5000
4000
3000
L 2000
1000
^ /L.
'!i":{i-:'
3.60 3.80 4.00 4.20 4.40 4.60 4.80 5.00 5.20 6.
--------
--
8-2 TBA--
space losses from water
[
:
Ir
10 mL. glass vial;
10mL water;
8-2 TBA at 150pg/L
120
tw100
2a
ey
20
|| 0 o 2 4 8 8 0 |
|
Time [hrs]
|
|i
[a] else]
ethod validation and sample
Experiment
Results (% r^overy st.
10 mi glass vial; 5 mi water;
8-2 TBA at 150
WA
Water Ihr
type RT
1 week
Frozen
Iweek
RT
Iweek
RT (No foil)
Well Pond
1026 982
Creek 996
Sea
962
985 916 865 865
6414 5712 536 929
354 302 298 298
- validation and sample stora
Results (% recovery ^t, dev.) 15|ig/L8-2TBA
Water Ihr
type RT
1 week Frozen
1 week
RT
Iweek
RT (no foil)
Well Pond
945 946
Creek 916
Sea 945
1084
----
---
----
284
---
----
----,
144
----
---
----
_1_5__p_g_/_L__8_-2__T__B-A^-h_i_s_S__e_a__w_a_t_e_r_
497
Ion 31.00 -8-2-TBA
4.00 4.50 5.00 5.50 6.00 6.50 7.00 7.50 8.00 8.50 9.00 9.50 ion 33.00 D-8-2 TBA
4.00 4.50 5,00 5.50 6.00 6.50 7.00 7.50 8.00 8.50 9.00 9.50
Extraction:
2 g soil, spike 8-2 TBA; add 1 mL H^O; extract with
6 mL hexane
Clean-up:
SPE: Si, 100 mg /10 mL (1ST)
1. 2 mL IPA and 2 mL Hexane
2. Load hexane extract 3. Wash with 6 mL hexane
4. Elute with 1 mL IPA
Results for 150 |ig/g s
Soil type
Poiazzo (44% sand, 26% slit,
30% clay)
Key Port (17% sand, 62% slit,
21% clay)
Hildago (52% sand, 20% slit,
28% clay)
White Clay (98% sand, 2% slit)
Soil
(% Rec.
stdev)
874
8815
8111 876
soil - chromatograms
Soils
Poiazzo soil extract
Ion 31 : 8-2 TBA
404550556065707580859095 -D
Ion 33 : D-8-2 TBA
40 45/50 55 60 65 70 75 80 85 90 95--D
Abutida.'lai 1000 900 800 700 600 SOO 400 300 200 100
TaTis-,-.
4.81 ^
Ion 95.00
jM)^^ ll
\i^niUV IVVt W^/V 'WT W OO 4so B-00 5-SO 6.00 6.50 7.00
^^
Vms--,
1400
. icn 95.00
1300 1200
K\ i-3.1
1100
1000
900
800
700
600
600
,Ji|Ljy 400
300
200 100
x-^^, --. -A.,^.-J- ^MMw\^
0
4-00
4.50
5.00
5.50
6-00
6,50
7.00
tissues procedures
Extraction:
0.3 g fat, (spike), dissolve
in 6 mL heptane
Clean-up:
SPE:Si,500mg/10mL
(1ST)
1. 1 mL acetone and 2 mL
heptane
2. Load heptane extract 3. Wash with 6 mL
heptane
4. Elute with 1 mL IPA
Extraction:
0.5 g tissue; (spike), add 2 mL water, 15 uL HC104; extract with 6 mL hexane; 15 min vortex; centrifuge
Clean-up:
SPE:Si,500mg/10mL
(1ST)
1. lmLIPAand2mL
hexane 2. Load hexane extract
3. Wash with 6 mL hexane 4. Elute with 1 mL IPA
Pl
Extr
0.25 mL mL water 15 min vo
s
No C
for
8-2 TBA - piaSma^andtissues chromatograms
Fat: 190 ng/g spike and blank
and tissues results
Matrix
Fat Liver Kidney Plasma
Spike Level
190 ng/g 950 ng/g 100 ng/g 200 ng/g 100 ng/g 100 ng/mL 200 ng/mL
8-2 TBA
(% Rec.
st.dev)
631 1003 984
805
725
867
11311
C9-iso
(% Rec.
st.dev)
6710 957 9715
799
7510
8215
10417
Estima
12 6.0 4.0 5.0
Summary
8-2 Telomer B alcohol is^<hallenging analyt because of its volatility and lov\^^ater solubilit
- low water solubility dictates the need fCT>n^
developed at LOQ;
^^^
- extraction solvent choice is critical in achieving re sensitivity, precision, and GC/MS system perfor
- volatility losses from water are rapid and significa
- solvent exchange is not an option, limiting the cho sample concentration or/and clean-up;
- samples should be stored frozen;
Summary
- demonstrated the analytfealprocedures for a
of 8-2 Telomer B alcohol in environmental wat
soils, rat plasma, and tissues;
N^
- extracts derived from complex matrices (sotktfesu
require clean-up;
\
- maintaining column performance is critical for reli quantitation and maintaining GC/MS sensitivity;
- use of internal standards (especially isotopically la
critical for accurate quantitation;
- use of surrogates is important for accurate quanti biological matrices;