Magnetic Solid-Phase Extraction Combined with Dispersive Liquid-Liquid Microextraction Followed by HPLC for Determination of Four Aromatic Amines Released from Azo Dyes in Paper Samples

Li, Xiaolan; Meng, Dongling; Liu, Ruiqi; Yang, Yaling

doi:10.21577/0103-5053.20170198

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Articles • J. Braz. Chem. Soc. 29 (4) • Apr 2018 • https://doi.org/10.21577/0103-5053.20170198 copy

Magnetic Solid-Phase Extraction Combined with Dispersive Liquid-Liquid Microextraction Followed by HPLC for Determination of Four Aromatic Amines Released from Azo Dyes in Paper Samples

Authorship SCIMAGO INSTITUTIONS RANKINGS

A novel extraction technique combining dispersive liquid-liquid microextraction (DLLME) with magnetic solid-phase extraction (MSPE) is presented for pre-concentration of four primary aromatic amines (PAAs) released from azo dyes in paper samples prior to high performance liquid chromatography (HPLC). n-Octanol was used as the extractant and hydrophobic oleic acid modified Fe₃O₄ nanoparticles (Fe₃O₄@OA NPs) as an efficient adsorbent was applied to retrieve the PAAs-containing n-octanol in the DLLME step. Because of the rapid mass transfer associated with the DLLME and MSPE steps, fast extraction could be achieved. The main parameters affecting the efficiency of MSPE-DLLME procedure of PAAs were investigated and optimized. Under optimum conditions, the recoveries ranged from 79.6 to 88.5% and the limits of detection (LODs) were in the range of 0.21-1.16 ng mL^-1 (S / N = 3). The intra-day precision (relative standard deviation (RSD)) was below 7.8% and inter-day RSD was less than 11%.

Keywords:
aromatic amines; magnetic solid-phase extraction; dispersive liquid-liquid microextraction; paper samples

Analyte	LDR^a a LDR: linear dynamic range; / (µg mL^-1)	Regression equation	R2 ^b b R2: square of correlation coefficient;	LOD^c c LOD: limit of detection. / (ng mL^-1)
2,4,5-Trimethylaniline	0.10-50	y = 40.611x - 0.5119	0.9988	1.16
p-Chloroaniline	0.10-50	y = 64.956x - 1.6193	0.9972	0.97
4-Aminobiphenyl	0.10-50	y = 10.205x + 4.5354	0.9969	0.21
p-Aminoazobenzene	0.10-50	y = 35.929x - 0.5443	0.9998	0.56

Concentration / (ng mL^-1)	Found (mean ± SD) / (ng mL^-1)	RSD (n= 6)
		Intra-day				Inter-day
		1	2	3	4	1	2	3	4
100	85.2 ± 1.5	5.8	7.2	7.8	5.2	6.5	10.3	9.7	6.9
300	255.6 ± 5.4	3.9	4.9	5.4	4.1	5.9	7.3	6.5	8.4
500	437 ± 13	5.2	3.6	3.7	6.5	8.2	5.9	5.4	10.6

Analyte	Spiked / (ng mL^-1)	Detected^a a The method of this work; / (ng mL^-1)		Detected^b b the method of Chinese National Standard; / (ng mL^-1)		Recovery^a a The method of this work; (n = 6) / %		RSD^a a The method of this work; ,^c c RSD: relative standard deviation. (1) Different cigarette papers; (2) different colored paper napkin samples. (n = 6) / %
Analyte	Spiked / (ng mL^-1)	1	2	1	2	1	2
p-Chloroaniline	0	0.97	0.97	0.97	0.97	-	-	-
	100	79.6	82.7	82.5	81.7	79.6	82.7	7.6
	500	426.5	402.4	420.7	401.9	85.3	80.4	5.8
2,4,5-Trimethylaniline	0	25.7	1.16	23.6	1.16	-	-	-
	100	111.3	84.3	109.4	83.7	88.5	84.3	4.9
	500	452.6	408.1	467.3	410.3	86.1	81.6	5.2
4-Aminobiphenyl	0	0.21	32.5	0.21	33.2	-	-	-
	100	82.3	109.3	79.5	111.4	82.3	82.5	4.7
	500	436	450.1	425.6	449.2	87.2	84.6	6.2
p-Aminoazobenzene	0	0.56	0.56	0.56	0.56	-	-	-
	100	85.7	88.2	86.3	87.6	85.7	88.2	5.1
	500	442	436.2	447.1	439	88.4	87.4	4.5

Analysis method	Matrix	Recovery / %	LR / (ng mL^-1)	Extraction time / min	LOD / (ng mL^-1)	Reference
MIL-DLLME-HPLC	vegetable oils	81.8-114.2	5.00-1000	7	1.31-1.49	¹1 Wang, Y.; Sun, Y.; Xu, B.; Li, X.; Jin, R.; Zhang, H.; Song, D.; J. Chromatogr. A 2014, 1373, 9.
HF-LLLME-HPLC	water samples	88.5-105.4	0.5-500	30	0.05-0.1	⁴⁴44 Zhao, L.; Zhu, L.; Lee, H. K.; J. Chromatogr. A 2002, 963, 239.
HF-LPME-HPLC	environmental water samples	80-103	5-200	80	0.5-1.5	⁴⁵45 Tao, Y.; Liu, J. F.; Wang, T.; Jiang, G. B.; J. Chromatogr. A 2014, 1216, 756.
IL-DLLME-HPLC	water samples	93.4-106.4	2-200	4	0.45-2.6	⁴⁶46 Fan, Y. C.; Hu, Z. L.; Chen, M. L.; Chao, S. T.; Zhu, Y.; Chin. Chem. Lett. 2008, 19, 985.
LLLME-HPLC	water	74.7-87.5	3-1000	20	0.8-1.80	⁴⁷47 Yazdi, A. S.; Es'haghi, Z.; Talanta 2005, 66, 664.
SPME-HPLC	water samples	55.3-104.7	5-5000	20	1.4-3.0	⁴⁸48 Knize, M. G.; Salmon, C. P.; Hopmans, E. C.; Felton, J. S.; J. Chromatogr. A 1997, 763, 179.
MSPE-DLLME-HPLC	paper samples	79.6-88.5	10-5000	2	0.21-1.16	this work

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