Determination of polybrominated diphenyl ethers in shrimp and animal origin oils in Medellín, Colombia

Figures & data

Table 1. Summary results of PBDE validation in shrimp and animal origin oils.

				Shrimp						Animal oil
Congener	RT	Target ion (Q1)	R^2 hexane	MDL ng·g^−1	MQL ng·g^−1	Level ng·g^−1	RSD (%)	REC (%)	R^2	MDL ng·g^−1	MQL ng·g^−1	Level ng·g^−1	RSD (%)	REC (%)	R^2
BDE-28	28.2	406 (404)	0.999	0.0014	0.0043	0.0050	25	77	0.999	0.0013	0.0039	0.0050	22	78	0.999
						0.50	18	85				0.50	17	79
						1.0	23	90				1.0	21	87
BDE-47	32.4	486 (484)	0.999	0.0013	0.0039	0.0050	24	86	0.999	0.0012	0.0036	0.0050	18	83	0.999
						0.50	11	87				0.50	15	80
						1.0	15	86				1.0	13	87
BDE-77	33.9	486 (484)	0.999	0.0016	0.0047	0.0050	18	83	0.999	0.0011	0.0033	0.0050	17	80	0.999
						0.50	24	83				0.50	20	78
						1.0	16	76				1.0	15	78
BDE-100	35.5	564 (566)	0.999	0.0013	0.0040	0.0050	14	79	0.999	0.0014	0.0042	0.0050	15	81	0.999
						0.50	14	91				0.50	16	84
						1.0	19	88				1.0	21	74
BDE-99	36.3	564 (566)	0.999	0.0015	0.0046	0.0050	20	77	0.999	0.0015	0.0045	0.0050	19	72	0.999
						0.50	11	77				0.50	13	79
						1.0	12	82				1.0	11	91
BDE-126	37.7	564 (566)	0.999	0.0013	0.0039	0.0050	17	83	0.999	0.0013	0.0039	0.0050	15	88	0.997
						0.50	19	84				0.50	18	87
						1.0	13	87				1.0	10	90
BDE-153	38.1	484 (482)	0.999	0.0013	0.0040	0.0050	14	86	0.999	0.0014	0.0042	0.0050	16	90	0.999
						0.50	14	82				0.50	14	78
						1.0	15	78				1.0	14	79
BDE-154	38.8	484 (482)	0.999	0.0011	0.0033	0.0050	13	79	0.998	0.0012	0.0036	0.0050	14	76	0.999
						0.50	16	91				0.50	16	92
						1.0	17	83				1.0	13	90
BDE-139	39.0	484 (482)	0.999	0.0012	0.0036	0.0050	18	91	0.999	0.0015	0.0045	0.0050	17	87	0.999
						0.50	18	89				0.50	18	85
						1.0	15	81				1.0	12	90
BDE-183	40.5	722 (562)	0.999	0.0012	0.0035	0.0050	14	89	0.999	0.0013	0.0039	0.0050	14	82	0.999
						0.50	22	79				0.50	23	81
						1.0	16	86				1.0	14	90

RT: Retention time, Target ion: Quantification ion (m/z), Q1: Confirmation ion (m/z), R²: Coefficient of determination, MDL: Estimated method detection limit, MQL: Estimated method quantification limit, RSD: Relative standard deviation, REC: Recovery percentage.

Figure 1. Evaluation of the matrix effect of BDE-47. Area in solvent vs area in matrix. CI: 95% confidence interval.

Table 2. U_exp (%) and polynomial model for the interpolation of the uncertainty of PBDEs in shrimp and animal origin oils.

	Shrimp		Animal oil
Congener	Polynomial model	Uexp máx (%)	Polynomial model	Uexp max (%)
BDE-28	y = 1.7x^2 – 5.2x + 44	44	y = −10x^2 + 3.2x + 47	47
BDE-47	y = 0.44x^2 – 6.1x + 46	46	y = 2.9 x^2 ^– 8.9x + 47	47
BDE-77	y = 8.0x^2 – 26x + 58	58	y = 7.2 x^2 – 26x + 59	59
BDE-100	y = 1.3x^2 – 3.7x + 47	47	y = −6.7 x^2 – 0.79x + 48	48
BDE-99	y = 1.7x^2 – 21x + 72	72	y = 4.2 x^2 ^– 25x + 70	70
BDE-126	y = 30x^2 – 55x + 65	65	y = 33 x^2 ^– 60x + 66	66
BDE-153	y = −17x^2 – 5.5x + 66	66	y = −11 x^2 ^– 14x + 68	68
BDE-154	y = −8.7x^2 + 0.78x + 57	57	y = −1.7 x^2 ^– 7.9x + 57	57
BDE-139	y = 23x^2 – 42x + 66	66	y = 24 x^2 ^– 45x + 66	66
BDE-183	y = 3.6x^2 – 12x + 50	50	y = 4.4 x^2 ^– 16x + 52	52

Figure 2. TIC chromatogram of shrimp samples. a: Solvent (n-hexane), b: Matrix blank, c: 0.050 ng·g⁻¹ standard, d: Spiked shrimp sample to 0.50 ng·g⁻¹, e: S4 shrimp sample.

Table 3. Results of PBDEs in shrimp samples (ng·g⁻¹).

	Sample concentration (ng·g^−1)
Congener	S1	S2	S3	S4	S5	S6	S7	S8	S9	S10
BDE-28	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050
BDE-47	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050
BDE-77	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050
BDE-100	<0.0050	<0.0050	<0.0050	0.012	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050
BDE-99	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050
BDE-126	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050
BDE-153	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050
BDE-154	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050
BDE-139	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050
BDE-183	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050

S1-S10: Shrimp samples, <0.005: Lower than lower reporting limit (ng·g⁻¹).

Figure 3. TIC chromatogram of animal oil samples. a: O1 sample, b: O3 sample, c: O5 sample.

Table 4. Results of PBDEs in animal origin oil samples (ng·g⁻¹).

	Sample concentration (ng·g^−1)
Congener	O1	O2	O3	O4	O5	O6	O7	O8	O9	O10
BDE-28	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050
BDE-47	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050
BDE-77	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050
BDE-100	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050
BDE-99	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050
BDE-126	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050
BDE-153	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050
BDE-154	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050
BDE-139	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050
BDE-183	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050	<0.0050

O1-O10: Animal origin oil samples, <0.005: Lower than lower reporting limit (ng·g⁻¹).