Chinese Journal of Chromatography ›› 2022, Vol. 40 ›› Issue (10): 889-899.DOI: 10.3724/SP.J.1123.2021.12032
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SUN Min, LI Chunying, SUN Mingxia, FENG Yang, FENG Jiaqing, SUN Haili, FENG Juanjuan()
Received:
2021-12-28
Online:
2022-10-08
Published:
2022-10-12
Contact:
FENG Juanjuan
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CLC Number:
SUN Min, LI Chunying, SUN Mingxia, FENG Yang, FENG Jiaqing, SUN Haili, FENG Juanjuan. Preparation and application of graphene oxide functionalized melamine-formaldehyde aerogel coated solid-phase microextraction tube[J]. Chinese Journal of Chromatography, 2022, 40(10): 889-899.
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URL: https://www.chrom-china.com/EN/10.3724/SP.J.1123.2021.12032
Fig. 2 Images of scanning electron microscopy (SEM) and X ray photoelectron spectroscopy (XPS) spectra of GO/MF aerogel-coated stainless steel wire a. SEM of GO/MF aerogel coated stainless steel wire (150 times); b. SEM of GO/MF aerogel coated stainless steel wire (50000 times); c. XPS spectrum of GO/MF aerogel; d. C 1s peak of XPS fine spectrum of GO/MF aerogel.
Fig. 3 Effect of functionalization of GO on extraction efficiencies of MF aerogel Nap: naphthalene; Acy: acenaphthylene; Ace: acenaphthene; Flu: fluorine; Phe: phenanthrene; Ant: anthracene; Fla: fluoranthene; Pyr: pyrene. Conditions: content of each analyte, 5.00 μg/L; sampling volume, 30 mL; sampling rate, 1.00 mL/min; desorption time, 2.0 min.
Fig. 4 Effect of extraction and desorption conditions on the extraction efficiencies a. sampling volume; b. sampling rate; c. volume fraction of methanol; d. desorption time.
Analyte | LOD/ (μg/L) | Enrichment factor | Linear range/ (μg/L) | Linear equation/ (μg/L) | r | RSDs (n=3)/% | |
---|---|---|---|---|---|---|---|
Intra-day | Inter-day | ||||||
Nap | 0.005 | 2295 | 0.017-20.0 | y=9.25×102c+1.96×103 | 0.9998 | 0.5 | 5.5 |
Acy | 0.005 | 2058 | 0.017-20.0 | y=4.57×102c+1.15×102 | 0.9996 | 0.9 | 5.2 |
Ace | 0.005 | 2208 | 0.017-20.0 | y=2.38×102c+1.39×101 | 0.9999 | 1.4 | 3.5 |
Flu | 0.005 | 2029 | 0.017-20.0 | y=8.50×102c+1.17×102 | 0.9996 | 0.9 | 2.9 |
Phe | 0.003 | 2542 | 0.010-20.0 | y=8.07×102c-5.37×101 | 0.9996 | 1.1 | 1.8 |
Ant | 0.003 | 2513 | 0.010-20.0 | y=2.03×103c-1.08×102 | 0.9995 | 1.5 | 6.0 |
Fla | 0.001 | 2668 | 0.003-15.0 | y=3.38×102c+2.69×101 | 0.9992 | 2.1 | 5.4 |
Pyr | 0.001 | 2875 | 0.003-15.0 | y=3.08×102c-9.63×101 | 0.9990 | 4.8 | 8.6 |
Table 1 LODs, enrichment factors, linear ranges, linear equations, correlation coefficients (r) and
Analyte | LOD/ (μg/L) | Enrichment factor | Linear range/ (μg/L) | Linear equation/ (μg/L) | r | RSDs (n=3)/% | |
---|---|---|---|---|---|---|---|
Intra-day | Inter-day | ||||||
Nap | 0.005 | 2295 | 0.017-20.0 | y=9.25×102c+1.96×103 | 0.9998 | 0.5 | 5.5 |
Acy | 0.005 | 2058 | 0.017-20.0 | y=4.57×102c+1.15×102 | 0.9996 | 0.9 | 5.2 |
Ace | 0.005 | 2208 | 0.017-20.0 | y=2.38×102c+1.39×101 | 0.9999 | 1.4 | 3.5 |
Flu | 0.005 | 2029 | 0.017-20.0 | y=8.50×102c+1.17×102 | 0.9996 | 0.9 | 2.9 |
Phe | 0.003 | 2542 | 0.010-20.0 | y=8.07×102c-5.37×101 | 0.9996 | 1.1 | 1.8 |
Ant | 0.003 | 2513 | 0.010-20.0 | y=2.03×103c-1.08×102 | 0.9995 | 1.5 | 6.0 |
Fla | 0.001 | 2668 | 0.003-15.0 | y=3.38×102c+2.69×101 | 0.9992 | 2.1 | 5.4 |
Pyr | 0.001 | 2875 | 0.003-15.0 | y=3.08×102c-9.63×101 | 0.9990 | 4.8 | 8.6 |
Fig. 5 (a) Durability and (b) chemical stability of GO/MF aerogel coated solid-phase microextraction tube Sampling volume: 70 mL; sampling rate: 2.00 mL/min; desorption time: 2.0 min.
Extraction material | Analytical method | LOD/(μg/L) | Linear range/ (μg/L) | Extraction time/min | Online/ offline test | ||
---|---|---|---|---|---|---|---|
GO/MF aerogel in this work | IT-SPME-HPLC-DAD | 0.001- | 0.005 | 0.010- | 20.0 | 35 | online |
SiO2 aerogel[ | IT-SPME-HPLC-DAD | 0.005- | 0.050 | 0.017- | 15 | 34 | online |
MF aerogel[ | IT-SPME-HPLC-DAD | 0.01- | 0.050 | 0.06- | 30 | 35 | online |
Melamine-formaldehyde-resorcinol aerogel[ | IT-SPME-HPLC-DAD | 0.01- | 0.050 | 0.03- | 30 | 33 | online |
Biocharcoal aerogel[ | IT-SPME-HPLC-DAD | 0.005- | 0.050 | 0.017- | 15 | 35 | online |
Magnetic metal-organic framework MIL-100(Fe) | MSPE-HPLC-FLD | 0.032- | 2.110 | 0.50- | 500 | 10 | offline |
microspheres[ | |||||||
Poly(9-vinylanthracene-co-ethylene dimethacrylate) | IT-SPME-HPLC-FLD | 0.00002- | 0.0002 | 0.0001- | 10 | 30 | online |
monolith[ | |||||||
Zeolitic imidazolate framework-8[ | IT-SPME-HPLC-FLD | 0.0005- | 0.005 | 0.01- | 5 | 25 | online |
Bamboo charcoal[ | SPE-HPLC-UVD | 0.011- | 0.087 | 0.2- | 15 | 8 | offline |
PDMS[ | HS-SPME-GC-MS | 0.01- | 0.5 | 0.05- | 200 | 90 | offline |
Table 2 Comparison to other analytical methods
Extraction material | Analytical method | LOD/(μg/L) | Linear range/ (μg/L) | Extraction time/min | Online/ offline test | ||
---|---|---|---|---|---|---|---|
GO/MF aerogel in this work | IT-SPME-HPLC-DAD | 0.001- | 0.005 | 0.010- | 20.0 | 35 | online |
SiO2 aerogel[ | IT-SPME-HPLC-DAD | 0.005- | 0.050 | 0.017- | 15 | 34 | online |
MF aerogel[ | IT-SPME-HPLC-DAD | 0.01- | 0.050 | 0.06- | 30 | 35 | online |
Melamine-formaldehyde-resorcinol aerogel[ | IT-SPME-HPLC-DAD | 0.01- | 0.050 | 0.03- | 30 | 33 | online |
Biocharcoal aerogel[ | IT-SPME-HPLC-DAD | 0.005- | 0.050 | 0.017- | 15 | 35 | online |
Magnetic metal-organic framework MIL-100(Fe) | MSPE-HPLC-FLD | 0.032- | 2.110 | 0.50- | 500 | 10 | offline |
microspheres[ | |||||||
Poly(9-vinylanthracene-co-ethylene dimethacrylate) | IT-SPME-HPLC-FLD | 0.00002- | 0.0002 | 0.0001- | 10 | 30 | online |
monolith[ | |||||||
Zeolitic imidazolate framework-8[ | IT-SPME-HPLC-FLD | 0.0005- | 0.005 | 0.01- | 5 | 25 | online |
Bamboo charcoal[ | SPE-HPLC-UVD | 0.011- | 0.087 | 0.2- | 15 | 8 | offline |
PDMS[ | HS-SPME-GC-MS | 0.01- | 0.5 | 0.05- | 200 | 90 | offline |
Analyte | Mineral water | Water from drinking fountain | |||||
---|---|---|---|---|---|---|---|
Content/(μg/L) | Added level/(μg/L) | Recovery/% | Content/(μg/L) | Added level/(μg/L) | Recovery/% | ||
Nap | N. D. | 1.00 | 98.1 | N. D. | 1.00 | 120.4 | |
5.00 | 99.7 | 5.00 | 107.5 | ||||
10.0 | 102.9 | 10.0 | 103.5 | ||||
Acy | N. D. | 1.00 | 78.7 | N. D. | 1.00 | 76.3 | |
5.00 | 91.7 | 5.00 | 94.8 | ||||
10.0 | 96.2 | 10.0 | 96.7 | ||||
Ace | N. D. | 1.00 | 90.1 | N. D. | 1.00 | 94.3 | |
5.00 | 92.6 | 5.00 | 97.6 | ||||
10.0 | 98.1 | 10.0 | 99.2 | ||||
Flu | N. D. | 1.00 | 86.2 | N. D. | 1.00 | 90.8 | |
5.00 | 91.1 | 5.00 | 95.2 | ||||
10.0 | 95.2 | 10.0 | 96.0 | ||||
Phe | N. D. | 1.00 | 97.3 | N. D. | 1.00 | 104.1 | |
5.00 | 94.8 | 5.00 | 100.8 | ||||
10.0 | 99.5 | 10.0 | 105.0 | ||||
Ant | N. D. | 1.00 | 95.3 | N. D. | 1.00 | 101.4 | |
5.00 | 97.2 | 5.00 | 103.7 | ||||
10.0 | 101.3 | 10.0 | 108.2 | ||||
Fla | N. D. | 1.00 | 84.0 | N. D. | 1.00 | 103.5 | |
5.00 | 106.3 | 5.00 | 116.9 | ||||
10.0 | 102.7 | 10.0 | 126.4 | ||||
Pyr | N. D. | 1.00 | 118.9 | N. D. | 1.00 | 120.8 | |
5.00 | 114.6 | 5.00 | 124.7 | ||||
10.0 | 105.1 | 10.0 | 132.8 |
Table 3 Spiked recoveries of the eight PAHs at three levels (n=3)
Analyte | Mineral water | Water from drinking fountain | |||||
---|---|---|---|---|---|---|---|
Content/(μg/L) | Added level/(μg/L) | Recovery/% | Content/(μg/L) | Added level/(μg/L) | Recovery/% | ||
Nap | N. D. | 1.00 | 98.1 | N. D. | 1.00 | 120.4 | |
5.00 | 99.7 | 5.00 | 107.5 | ||||
10.0 | 102.9 | 10.0 | 103.5 | ||||
Acy | N. D. | 1.00 | 78.7 | N. D. | 1.00 | 76.3 | |
5.00 | 91.7 | 5.00 | 94.8 | ||||
10.0 | 96.2 | 10.0 | 96.7 | ||||
Ace | N. D. | 1.00 | 90.1 | N. D. | 1.00 | 94.3 | |
5.00 | 92.6 | 5.00 | 97.6 | ||||
10.0 | 98.1 | 10.0 | 99.2 | ||||
Flu | N. D. | 1.00 | 86.2 | N. D. | 1.00 | 90.8 | |
5.00 | 91.1 | 5.00 | 95.2 | ||||
10.0 | 95.2 | 10.0 | 96.0 | ||||
Phe | N. D. | 1.00 | 97.3 | N. D. | 1.00 | 104.1 | |
5.00 | 94.8 | 5.00 | 100.8 | ||||
10.0 | 99.5 | 10.0 | 105.0 | ||||
Ant | N. D. | 1.00 | 95.3 | N. D. | 1.00 | 101.4 | |
5.00 | 97.2 | 5.00 | 103.7 | ||||
10.0 | 101.3 | 10.0 | 108.2 | ||||
Fla | N. D. | 1.00 | 84.0 | N. D. | 1.00 | 103.5 | |
5.00 | 106.3 | 5.00 | 116.9 | ||||
10.0 | 102.7 | 10.0 | 126.4 | ||||
Pyr | N. D. | 1.00 | 118.9 | N. D. | 1.00 | 120.8 | |
5.00 | 114.6 | 5.00 | 124.7 | ||||
10.0 | 105.1 | 10.0 | 132.8 |
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