Quantification of brominated flame retardants in soil

	Name	CAS No.	Acronym	m/z
nBFR	2,3,5,6-Tetrabromo-p-xylene	23488-38-2	TBX	419.7182 421.7162
	2,3,4,5,6-Pentabromotoluene	87-83-2	PBT	491.6307 499.6282
	2,3,4,5,6-Pentabromoethylbenzene	85-22-3	PBEB	485.6105 487.6085
	Hexabromobenzene	87-82-1	HBB	547.5074 549.5054
	2-Ethylhexyl 2,3,4,5-tetrabromobenzoate	183658-27-7	EH-TBB	418.6735 420.6714
	1,2-Bis(2,4,6-tribromophenoxy)ethane	37853-59-1	BTBPE	356.7948 358.7928
	Bis(2-ethylhexyl) tetrabromophthalate	26040-51-7	BEH-TBPH	462.6633 464.6613
	1,2-Bis(2,3,4,5,6-pentabromophenyl)ethane	84852-53-9	DBDPE	484.6032 486.6000
	2,4,4′-2,4,4′-Tribromodiphenylether	41318-75-6	BDE-28	405.8027 407.8002
PBDE	2,2′,4,4′-Tetrabromodiphenyl ether	5436-43-1	BDE-47	483.7132 485.7111
	2,2′,4,5′-Tetrabromodiphenyl ether	243982-82-3	BDE-49	483.7132 485.7111
	2,2′,4,4′,5-Pentabromodiphenyl ether	60348-60-9	BDE-99	492.9691 563.6216
	2,2′,4,4′,6-Pentabromodiphenyl ether	189084-64-8	BDE-100	492.9691 563.6216
	2,2,3,4,4,5-Hexabromodiphenyl ether	67888-98-6	BDE-138	481.6980 483.6960
	2,2′,4,4′,5,5′-Hexabromodiphenyl ether	68631-49-2	BDE-153	481.6980 483.6960
	2,2′,4,4′,5,6′-Hexabromodiphenyl ether	207122-15-4	BDE-154	481.6980 483.6960
	2,2′,3,4,4′,5′,6-Heptabromodiphenyl ether	207122-16-5	BDE-183	561.6060 563.6040
	Decabromodiphenyl ether	1163-19-5	BDE-209	799.3330 801.3310

Table 2.

Validation results of the developed method for polybrominated diphenyl ether quantification in soil

	BDE-28	BDE-47	BDE-49	BDE-99	BDE-100	BDE-138	BDE-153	BDE-154	BDE-183	BDE-209
LOD (ng/g d.m.)	0.0005	0.005	0.003	0.002	0.001	0.0006	0.0006	0.002	0.003	0.05
LOQ (ng/g d.m.)	0.002	0.016	0.009	0.006	0.004	0.002	0.002	0.005	0.011	0.15
Level 1
Fortification (ng/g d.m.)	2.0	2.0	2.0	2.0	2.0	3.0	3.0	3.0	3.0	10.0
Repeatability
Trueness (%)	10	8	1	11	11	8	6	9	12	5
CV (%)	4.3	7.0	6.4	7.7	7.4	5.7	6.1	4.9	8.2	3.8
Reproducibility
Trueness (%)	6.0	3.6	–2.2	4.4	5.1	4.3	2.4	4.5	5.9	4.9
CV (%)	5.1	6.5	5.7	8.7	8.1	5.7	5.9	5.6	8.6	3.1
Uncertainty (%)	64	25	21	27	28	26	25	22	59	32
Level 2
Fortification (ng/g d.m.)	4.0	4.0	4.0	4.0	4.0	6.0	6.0	6.0	6.0	20
Trueness (%)	5	4	2	6	7	6	3	6	9	2
CV (%)	4.1	5.5	8.8	4.5	4.0	2.1	2.8	1.6	6.0	6.8
Uncertainty (%)	64	23	29	22	24	15	21	19	57	34
Level 3
Fortification (ng/g d.m.)	100	100	100	100	100	150	150	150	150	500
Trueness (%)	–3	–14	–18	–14	–13	–12	–13	–11	–14	–11
CV (%)	7.4	1.7	12.3	3.3	4.1	1.4	3.4	1.5	4.3	6.2
Uncertainty (%)	65	19	52	21	24	27	22	19	56	34
Linearity
R²	1.0000	0.9994	0.9999	0.9999	0.9999	1.0000	1.0000	1.0000	0.9999	1.0000
β₁	0.965	0.868	0.814	0.852	0.861	0.875	0.865	0.883	0.852	0.884
β₀	0.196	–0.352	0.402	0.443	0.443	0.565	0.515	0.548	0.730	1.429

1 BDE – brominated diphenyl ether; LOD – limit of detection; LOQ – limit of quantification; Level 1/2/3 – enrichment levels; d.m. – dry matter; CV – coefficient of variation; R² – coefficient of determination; β₀ and β₁ – are dimensional parameter vector in the equation y=β₀ + β1x

Table 3.

Validation results of the developed method for novel brominated flame retardant quantification in soil

	TBX	PBT	PBEB	HBB	EH-TBB	BTBPE	BEH-TBPH	DBDPE
LOD (ng/g d.m.)	0.0007	0.001	0.001	0.002	0.018	0.0014	0.005	0.005
LOQ (ng/g d.m.)	0.002	0.004	0.003	0.005	0.061	0.005	0.018	0.015
Level 1
Fortification (ng/g d.m.)	0.050	0.050	0.20	0.050	0.20	0.20	0.50	1.0
Repeatability
Trueness (%)	14	0	1	12	2	1	7	7
CV (%)	7.5	9.5	7.1	8.8	6.4	3.5	6.2	11.7
Reproducibility
Trueness (%)	6.4	7.3	8.2	10.1	4.9	4.3	8.5	16.0
CV (%)	17	2	–5	18	1	3	3	0
Uncertainty (%)	18	30	23	39	22	13	27	40
Level 2
Fortification (ng/g d.m.)	1.00	1.00	4.0	1.0	4.0	4.0	10.0	20
Trueness (%)	–4	–11	–7	3	–10	–5	–2	33
CV (%)	2.9	4.6	4.6	6.4	3.7	2.8	5.2	2.8
Uncertainty (%)	14	28	22	22	25	15	18	68
Level 3
Fortification (ng/g. d.m.)	25	25	100	25	100	100	250	505
Trueness (%)	–7	–9	–18	–2	5	–9	–11	–22
CV (%)	5.2	6.6	3.3	4.9	6.4	5.2	8.6	19.6
Uncertainty (%)	23	28	40	17	24	25	36	71
Linearity
R²	1.00000	1.00000	0.99997	1.00000	0.99997	1.00000	0.99998	0.99928
β₁	0.927	0.911	0.817	0.974	1.047	0.912	0.885	0.776
β₀	0.014	–0.005	0.158	0.022	–0.187	0.062	0.343	3.710

1 TBX – 2,3,5,6-tetrabromo-p-xylene; PBT – 2,3,4,5,6-pentabromotoluene; PBEB – 2,3,4,5,6-pentabromoethylbenzene; HBB – hexabromobenzene; EH-TBB – 2-ethylhexyl 2,3,4,5-tetrabromobenzoate; BTBPE – 1,2-bis(2,4,6-tribromophenoxy)ethane; BEH-TBPH – bis(2-ethylhexyl) tetrabromophthalate; DBDPE – 1,2-bis(2,3,4,5,6-pentabromophenyl)ethane; LOD – limit of detection; LOQ – limit of quantification; Level 1/2/3 – enrichment levels; d.m. – dry matter; CV – coefficient of variation; R² – coefficient of determination; β₀ and β₁ – are dimensional parameter vector in the equation y=β₀ + β1x

Table 4.

Validation results of the developed procedure for PBDEs’ (polybrominated diphenyl ethers) and nBFRs’ (novel brominated flame retardants sums in soil

	$\sum PBDE$ without BDE-209	$\sum PBDE$	$\sum nBFR$ without DBDPE	$\sum nBFR$	$\sum BFR$
LOD (ng/g. d.m.)	0.014	0.049	0.022	0.022	0.057
LOQ (ng/g d.m.)	0.045	0.162	0.072	0.072	0.192
Level 1
Fortification (ng/g. d.m.)	24	34	1.3	2.3	36
Repeatability
Trueness (%)	9	7	5	6	7
CV (%)	6.2	5.4	1.2	5.0	5.1
Reproducibility
Trueness (%)	–1	1	3	2	1
CV (%)	0.7	0.9	3.6	7.9	5.1
Uncertainty (%)	27	23	12	21	23
Level 2
Fortification (ng/g. d.m.)	48	68	25	45	113
Trueness (%)	5	4	–5	12	7
CV (%)	3.6	4.2	3.6	2.9	3.0
Uncertainty (%)	16	16	15	27	19
Level 3
Fortification (ng/g. d.m.)	1200	1700	625	1130	2830
Trueness (%)	–13	–12	–9	–15	–13
CV (%)	0.9	2.0	4.5	8.8	2.6
Uncertainty (%)	26	26	23	40	28
R²	0.99995	0.99996	1.00000	0.99986	0.99993
β₀	0.87	0.87	0.91	0.85	0.86
β₁	4.58	6.01	0.41	4.12	10.24

1 $\sum PBDE$ – sum of polybrominated diphenyl ethers; $\sum nBFR$ – sum of novel brominated flame retardants; DBDPE – 1,2-Bis(2,3,4,5,6-pentabromophenyl)ethane; $\sum BFR$ – sum of brominated flame retardants; LOD – limit of detection; LOQ – limit of quantification; Level 1/2/3 – enrichment levels; d.m. – dry matter; CV – coefficient of variation; R² – coefficient of determination; β₀ and β₁ – are dimensional parameter vector in the equation y=β₀ + β₁x

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DOI: https://doi.org/10.2478/jvetres-2025-0070 | Journal eISSN: 2450-8608 (formerly 2300-3235)

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Language: English

Page range: 581 - 589

Submitted on: Aug 9, 2025

Accepted on: Dec 4, 2025

Published on: Dec 10, 2025

Published by: National Veterinary Research Institute in Pulawy

In partnership with: Paradigm Publishing Services

Keywords:

brominated flame retardants,

method development,

nBFRs,

PBDEs,

soil contamination

Related subjects:

Life sciences,

Molecular biology,

Microbiology and virology,

Life sciences, other,

Medicine,

Veterinary medicine

© 2025 Wojciech Jerzy Pietroń, Monika Baran, Marek Pajurek, Szczepan Mikołajczyk, published by National Veterinary Research Institute in Pulawy
This work is licensed under the Creative Commons Attribution 4.0 License.

Volume 69 (2025): Issue 4 (December 2025)