FLAME RETARDANT TEXTILE FINISHING CHEMICALS: IN VITRO ASSESSMENT OF DERMAL ABSORPTION - Meritxell Martí, Cristina Alonso, Albert Manich, Luisa ...
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FLAME RETARDANT TEXTILE
FINISHING CHEMICALS: IN VITRO
ASSESSMENT OF DERMAL
ABSORPTION
Meritxell Martí, Cristina Alonso, Albert Manich, Luisa Coderch
Institute of Advanced Chemistry of Catalonia, IQAC-CSIC, Barcelona, Spain
INTRODUCTION
Life‐FLAREX aims to carry out an analysis of
the environmental impact of the best technologies currently available
that are alternative to toxic flame retardants (FR) used in textile finishing processes.
The project will concentrate on those that are halogenated, contain antimony or are
formaldehyde‐releasing, and demonstrate which are the best alternatives: the less toxic,
with low environmental impact but at the same time those that keep the required
properties of the fabric.
MITIGATION OF ENVIRONMENTAL IMPACT
CAUSED BY FLAME RETARDANT TEXTILE
FINISHING CHEMICALS
www.life-flarex.eu
Fabric selection
PREPARATION Market study
FR used in different applications
Lab-scale
FR
DEMONSTRATION
application Industrial scale in 6 textile companies
Environmental Impact: LCA
IMPACTS Risk Assessment
In-vitro assessment toxicological potential
Technical Workshops for textile industry
AWARNESS RAISING Policy Recomendations
Road Map
PREPARATION: MATERIALS SELECTION Ö Fabrics
Upholstery Mattress ticking
Bedding sheets Curtains
Cotton
Polyester
Cotton/polyester
PREPARATION: MATERIALS SELECTION Ö FR Products
A1) (phosphorous based
C1) Decabromo diphenyl ethane
polymers)phosphate-phosphinate
(DecaBDE) + melamine cyanurate
A2) Expandable graphite
C2) DecaBDE + antimony trioxide
A3) Melamine encapsulated APP
(ATO)
A4) Guanidine Phosphate
C3) Dialkyl phosphono carboxylic acid
A5) Ammonium sulphamate
amide
A6) Ammonium Sulfamate +Urea
+PO(OH)2-R-PO(OH)2)
I1) Brominated polymer A7) Phosphonate aqueous solution
IN-VITRO ASSESSMENT TOXICOLOGICAL POTENTIAL
AIM: it is focused on dermal absorption of FR.
Until now, no studies were found about the textile release of FR to the skin in
contact with them. The growing evidence that suggests dermal absorption to be
potentially significant pathway of human exposure to FRs, supports the interest in
the study of percutaneous absorption of the FR.
FR selection Î skin contact at its final application
Optimization of analytical methodology using HPLC‐DAD for FR products
Percutaneous Ansorption Assay of FR products
Determination of Margin of Safety of each FR applied on textiles
IN-VITRO ASSESSMENT TOXICOLOGICAL POTENTIAL
Mattress ticking
Bedding sheets
2 ALTERNATIVE FLAME RETARDANT COMERCIAL PRODUCTS
Application by fulard:
AMMONIUM SULAFAMATE
FR code Composition Textile code Description
PES/CO 50/50 mattress ticking
Flarex004‐047
treated (pick‐up 11 wt%) with FR A
FR A Ammonium sulfamate
IN-VITRO ASSESSMENT TOXICOLOGICAL POTENTIAL
Optimization of analytical methodology using HPLC‐DAD for FR products
Standard samples of Ammonium Sulfamate (AS) at different concentration
(in the range 0.390-486 µg/mL) were analyzed by HPLC-DAD.
DAD1 A, Sig=390,60 Ref=310,8 (Cristina_A..._Calibracio_PELL 2018-11-12 15-47-15\025-D1F-B9-ST SALF 486.D)
mAU
80
60 retention time of 6.1 min
40
78
.8
A6r . 4 0 2
97
:7
ea
20
0
-20
2 4 6 8 10 12 14 16 18 min
Calibration curve for Ammonium Sulfamate:
900 y = 1,5428x + 74,472 Linearity range: 6.2‐ 486 µg/mL
800 R² = 0,9907
700 Calibration curve: Y= 1.54X‐74.47 R²>0.99
600
500 Limit of Detection (LOD): 2.05 µg/mL
Area
400
300 Limit of quantification (LOQ): 6.21 µg/mL
200
100 Intra‐day variation (CV): 0.11 %
0
0,00 100,00 200,00 300,00 400,00 500,00 600,00 Inter‐day variation (CV): 6.50%
Conc (µg/mL)
IN-VITRO ASSESSMENT TOXICOLOGICAL POTENTIAL
Concentration of ammonium sulfamate in each FR formulation, and
amount of ammonium sulfamate on each treated sample:
SAMPLE % Conc (w/w) % wt textile
FR A 40.03±2.51 -
FR B 37.19±0.36 -
Flarex002-2(CO) - 7.58 ± 1.65
Flarex004-035 (PES) - 14.50 ± 1.52
Flarex004-047 (PES/CO) - 11.13 ± 0.64
FR A FR B
IN-VITRO ASSESSMENT TOXICOLOGICAL POTENTIAL
Percutaneous Ansorption Assay of FR products
Intact pig skin discs:
• thickness: 500 µm
• diameter: 2.6 cm
Franz type static diffusion cell:
TEWL measurement
¾ exposure area: 1.86 cm2 (barrier integrity)
¾ receptor volume: 3 ml and skin temperature
¾ in a thermostated bath (32ºC)
IN-VITRO ASSESSMENT TOXICOLOGICAL POTENTIAL
Percutaneous Ansorption Assay of FR products
Pieces of non-treated and treated Franz diffusion cells with treated textiles
textiles to extract before analysis by during percutaneous absorption .
HPLC-DAD.IN-VITRO ASSESSMENT TOXICOLOGICAL POTENTIAL
Percutaneous Ansorption Assay of FR products
In vitro percutaneous absorption of ammonium sulfamate
from treated textiles.
(T: rest on fabric, SC: stratum corneum; E: epidermis; D:
dermis; Fluid R. receptor fluid: R: scrap).
% 035_PES FR A 047_PES/COFR A 2_co FR B
T 10939,00 3751,11 2601,22
SC 64,68 41,92 30,61
E 8,68 0,00 17,29
D b.l.q b.l.q b.l.q
Fluid R b.l.q b.l.q b.l.q
R 819,52 932,75 437,99
TOTAL 11116,71 4725,78 2873,92
Perc.Abs. 8,68±15,03 0,00 17,29± 2,05
b.l.q. below limit of quantifyIN-VITRO ASSESSMENT TOXICOLOGICAL POTENTIAL
Percutaneous Ansorption Assay of FR products
2 CO FR A
035 PES FR B
047 PES/CO FR B
Mass balance accepted (100±15%)
2 CO FR A: present in E
035PES FR B: present in E
047 PES/CO FR B: no detection in E, D, RFIN-VITRO ASSESSMENT TOXICOLOGICAL POTENTIAL
Determination of Margin of Safety of each FR applied on textiles
NOAEL is defined as the
Margin of Safety (MoS) highest dose or exposure level
where no (adverse) treatment-
NOAEL related findings are observed.
MoS=
SED SED: systemic exposure
doseIN-VITRO ASSESSMENT TOXICOLOGICAL POTENTIAL
Determination of Margin of Safety of each FR applied on textiles
Margin of Safety (MoS)
NOAEL
MoS= 100 NO TOXIC
SED
SSA = 15670 cm2 (Ö Body lotion: body-head)
F= 1day-1
2 CO FR B 035 PES FR A 047 PES/CO FR A
Daa (μg/cm2) 17,29 8,68 0,00
SED (mg/kg bw/d) 4,515 2,267 -
NOAEL (mg/ kg bw/d) 1000 1000 -
MoS 221,5 441,1 -IN-VITRO ASSESSMENT TOXICOLOGICAL POTENTIAL The FR based on ammonium sulfamate: - can penetrate via dermal pathway into skin, - but only a low levels, - so it isn’t toxic. COTTON POLYESTER PES/CO 50/50 Bed linen Mattress ticking Mattress ticking
IN-VITRO ASSESSMENT TOXICOLOGICAL POTENTIAL In this study, the possible topical dermal route for textile finishing products from fabric was demonstrated in the particular case of flame retardant product based on ammonium sulfamate: • The percutaneous absorption experiments demonstrated that topical friction of this textiles permit the active compound penetration until epidermis for both commercial products, for cotton with 15% of ammonium sulfamate (FR B) and for PES with 40% of ammonium sulfamate (FR A). However, the percutaneous absorption were very small, between 0.06% and 0.63% of ammonium sulfamate applied on the textiles. • The risk characterization of these alternative flame retardant products for finishing textile industry, calculating the Margin of Safety (MoS) of ammonium sulfamate, demonstrated that these FR products are not toxic.
meritxell.marti@iqac.csic.es Acknowledgement: Authors wish to thank the LIFE Environmental Policy and Governance program from the European Union for its financial contribution to the LIFE-FLAREX (LIFE16 ENV/ES/000374) project
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