Fabrication and application of polyaniline/titanium dioxide nanotube solid phase microextraction fiber

doi:10.3724/SP.J.1123.2019.10012

Abstract

Abstract:

A novel solid phase microextraction fiber of polyaniline coated titania composite nanotube (PANI@TiO₂NTs/Ti) array was fabricated on a titanium wire by in situ oxidation. The effects of the inorganic acid medium, aniline concentration, and oxidation voltage on the electropolymerization of aniline were discussed. The best forming conditions for the composite fiber obtained by analyzing the surface morphology and composition of the fibers were as follows:electrolyte composing, 0.5 mol/L aniline-1 mol/L H₂SO₄; electropolymerization, 10 V for 60 min. The developed fibers were used in conjunction with high performance liquid chromatography for the extraction and determination of ultraviolet filters in samples, and the extraction conditions optimized were as follows:extraction time 40 min, desorption time 4 min, extraction temperature 40℃, stirring rate 600 r/min. The average recoveries of the target analytes spiked in real samples ranged from 78.2% to 118%, and the relative standard deviations ranged from 4.4% to 8.9%. The developed method is simple, rapid, and accurate, and it is suitable for the sensitive determination of UV filters in environmental water samples.

Key words: solid phase microextraction (SPME), high performance liquid chromatography (HPLC), ultraviolet filters, titanium dioxide, polyaniline

MA Mingguang, WEI Yunxia, LIU Haixia, LIU Fang, SHANG Qiong. Fabrication and application of polyaniline/titanium dioxide nanotube solid phase microextraction fiber[J]. Chinese Journal of Chromatography, 2020, 38(6): 639-646.

Figures/Tables 9

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UV filter	Linear range/ (μg/L)	R²	LOD/(μg/L)	LOQ/(μg/L)	RSDs/%^*
UV filter	Linear range/ (μg/L)	R²	LOD/(μg/L)	LOQ/(μg/L)	Single fiber (n=5)	Fiber-to-fiber (n=3)
* Calculated at the mass concentration of 25 μg/L.
BP-3	0.25-500	0.9998	0.05	0.19	4.7	7.6
OD-PABA	0.25-500	0.9987	0.05	0.18	5.7	8.8
EHMC	0.25-500	0.9992	0.04	0.14	4.3	6.9
EHS	0.25-500	0.9953	0.06	0.22	5.3	9.3

UV filter	Linear range/ (μg/L)	R²	LOD/(μg/L)	LOQ/(μg/L)	RSDs/%^*
UV filter	Linear range/ (μg/L)	R²	LOD/(μg/L)	LOQ/(μg/L)	Single fiber (n=5)	Fiber-to-fiber (n=3)
* Calculated at the mass concentration of 25 μg/L.
BP-3	0.25-500	0.9998	0.05	0.19	4.7	7.6
OD-PABA	0.25-500	0.9987	0.05	0.18	5.7	8.8
EHMC	0.25-500	0.9992	0.04	0.14	4.3	6.9
EHS	0.25-500	0.9953	0.06	0.22	5.3	9.3

Sample	Analyte	Background/ (μg/L)	Spiked with 5 μg/L			Spiked with 10 μg/L
Sample	Analyte	Background/ (μg/L)	Detected/ (μg/L)	Recovery/ %	RSD/ %	Detected/ (μg/L)	Recovery/ %	RSD/ %
^a ND: not detected or lower than LOD.
River water under Bapanxia Bridge	BP-3	0.62	5.96	106	4.4	9.34	88.0	6.7
	OD-PABA	0.84	6.82	117	5.6	12.8	118	7.2
	EHMC	0.96	6.45	108	4.4	9.98	91.1	5.8
	EHS	ND^a	4.86	97.2	7.0	9.63	96.3	7.9
River water under Yintan Bridge	BP-3	3.08	7.52	93.1	5.5	12.6	96.3	6.7
	OD-PABA	2.89	8.73	111	6.0	13.5	105	7.3
	EHMC	1.28	6.64	106	5.1	13.0	115	6.8
	EHS	ND	5.40	108	7.9	7.82	78.2	8.5
River water under Zhongshan Bridge	BP-3	1.82	6.27	91.9	5.5	10.4	88.0	6.5
	OD-PABA	2.01	6.36	90.7	5.9	11.6	96.6	7.1
	EHMC	2.52	6.49	86.3	4.7	14.0	112	5.7
	EHS	ND	4.51	90.2	8.3	10.8	108	7.9
River water under Donggang Bridge	BP-3	2.28	6.96	95.6	5.0	13.4	109	5.3
	OD-PABA	2.16	8.44	118	5.2	12.0	98.7	6.3
	EHMC	2.10	6.82	96.1	4.6	13.5	112	5.9
	EHS	ND	5.18	104	7.6	11.0	102	8.5
River water under Shichuan Bridge	BP-3	2.02	6.54	93.2	5.0	13.3	111	6.1
	OD-PABA	2.54	6.78	89.9	5.6	14.1	112	6.8
	EHMC	1.02	6.64	110	5.0	10.6	96.2	5.9
	EHS	ND	4.87	97.4	8.2	10.6	106	8.4
Wastewater	BP-3	2.83	6.87	87.74	5.7	13.6	106	6.6
	OD-PABA	3.52	7.23	84.86	6.1	15.2	112	7.1
	EHMC	2.17	6.52	90.93	5.0	13.5	111	6.9
	EHS	ND	4.62	92.40	7.3	9.07	90.7	8.9

Sample	Analyte	Background/ (μg/L)	Spiked with 5 μg/L			Spiked with 10 μg/L
Sample	Analyte	Background/ (μg/L)	Detected/ (μg/L)	Recovery/ %	RSD/ %	Detected/ (μg/L)	Recovery/ %	RSD/ %
^a ND: not detected or lower than LOD.
River water under Bapanxia Bridge	BP-3	0.62	5.96	106	4.4	9.34	88.0	6.7
	OD-PABA	0.84	6.82	117	5.6	12.8	118	7.2
	EHMC	0.96	6.45	108	4.4	9.98	91.1	5.8
	EHS	ND^a	4.86	97.2	7.0	9.63	96.3	7.9
River water under Yintan Bridge	BP-3	3.08	7.52	93.1	5.5	12.6	96.3	6.7
	OD-PABA	2.89	8.73	111	6.0	13.5	105	7.3
	EHMC	1.28	6.64	106	5.1	13.0	115	6.8
	EHS	ND	5.40	108	7.9	7.82	78.2	8.5
River water under Zhongshan Bridge	BP-3	1.82	6.27	91.9	5.5	10.4	88.0	6.5
	OD-PABA	2.01	6.36	90.7	5.9	11.6	96.6	7.1
	EHMC	2.52	6.49	86.3	4.7	14.0	112	5.7
	EHS	ND	4.51	90.2	8.3	10.8	108	7.9
River water under Donggang Bridge	BP-3	2.28	6.96	95.6	5.0	13.4	109	5.3
	OD-PABA	2.16	8.44	118	5.2	12.0	98.7	6.3
	EHMC	2.10	6.82	96.1	4.6	13.5	112	5.9
	EHS	ND	5.18	104	7.6	11.0	102	8.5
River water under Shichuan Bridge	BP-3	2.02	6.54	93.2	5.0	13.3	111	6.1
	OD-PABA	2.54	6.78	89.9	5.6	14.1	112	6.8
	EHMC	1.02	6.64	110	5.0	10.6	96.2	5.9
	EHS	ND	4.87	97.4	8.2	10.6	106	8.4
Wastewater	BP-3	2.83	6.87	87.74	5.7	13.6	106	6.6
	OD-PABA	3.52	7.23	84.86	6.1	15.2	112	7.1
	EHMC	2.17	6.52	90.93	5.0	13.5	111	6.9
	EHS	ND	4.62	92.40	7.3	9.07	90.7	8.9

Method	Extraction time/min	Linear range/(μg/L)	LOD/(μg/L)	RSD/%	Recovery/%	Ref.
CPE: cloud point extraction; SDME: single drop microextraction; HF-LPME: hollow fiber liquid phase microextraction; DLLME: dispersive liquid-liquid microextraction; MSA-DLLME magnetic stirring assisted dispersive liquid-liquid microextraction.
CPE	30	0.5-30	0.14-1.27	3.9-5.2	98.5-102	[28]
SDME	37	1-300	0.06-3.0	2.8-7.9	92-115	[29]
HF-LPME	50	5-1000	0.2-0.5	1.1-8.4	95.2-105	[30]
DLLME	10	0.5-500	0.06-0.16	2.8-7.6	92.8-114	[31]
MSA-DLLME	25	5-20000	0.2-0.8	1.4-4.8	91.3-97.1	[32]
SPME	40	0.25-500	0.04-0.06	4.3-8.9	90.6-110	this method