Chinese Journal of Chromatography ›› 2020, Vol. 38 ›› Issue (9): 1095-1101.DOI: 10.3724/SP.J.1123.2020.02031
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ZHAO Lingyi, LÜ Wenjuan(), NIU Xiaoying, PAN Congjie, CHEN Hongli, CHEN Xingguo()
Received:
2020-03-06
Online:
2020-09-08
Published:
2020-12-11
Contact:
LÜ Wenjuan,CHEN Xingguo
Supported by:
ZHAO Lingyi, LÜ Wenjuan, NIU Xiaoying, PAN Congjie, CHEN Hongli, CHEN Xingguo. Preparation of a two-dimensional azine-linked covalent organic framework-coated capillary and its application to the separation of nitrophenol environmental endocrine disruptors by open-tubular capillary electrochromatography[J]. Chinese Journal of Chromatography, 2020, 38(9): 1095-1101.
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URL: https://www.chrom-china.com/EN/10.3724/SP.J.1123.2020.02031
Fig. 2 (a) X-ray powder diffraction (XRD) pattern of the synthesized ACOF-1 and (b) FT-IR spectra of the synthesized ACOF-1 (Ⅰ) and the ACOF-1 coated capillary (Ⅱ)
Fig. 4 Typical electropherogram of four nitrophenol analytes with the ACOF-1 coated capillary Buffer solution: 15 mmol/L borate with 10% (v/v) CH3OH, pH 9.20. Applied voltage: -23 kV. Detection wavelength: 214 nm. Capillary: 50.2 cm total length (40.0 cm effective length).Peak identification: 1.2-nitrophenol (2-NP); 2.4-nitrophenol (4-NP); 3.2,4-dinitrophenol (DNP); 4.2,4,6-trinitrophenol (TNP).
Analyte | N/(plates/m) | Linear range/(mg/L) | Linear equation | R2 | LOD/(mg/L) | LOQ/(mg/L) |
y: peak area (AU\5min); x: mass concentration of analytes, mg/L. LOD: calculated on the basis of 3s/k (s: the deviation of baseline; k: the slope of the linear equation). LOQ: calculated on the basis of 10s/k. | ||||||
2-NP | 21514 | 10-500 | y=4399.46x+10176.18 | 0.9977 | 0.13 | 0.45 |
4-NP | 20529 | 10-500 | y=2575.18x+25294.24 | 0.9998 | 0.23 | 0.76 |
DNP | 17352 | 20-1000 | y=2881.43x+71.93 | 0.9975 | 0.20 | 0.68 |
TNP | 11262 | 20-1000 | y=3283.97x+6775.26 | 0.9959 | 0.18 | 0.60 |
Table 1 Column efficiencies (N), linear ranges, linear equations, determination coefficients (R2), limits of detection (LODs) and limits of quantification (LOQs) for the four nitrophenol analytes
Analyte | N/(plates/m) | Linear range/(mg/L) | Linear equation | R2 | LOD/(mg/L) | LOQ/(mg/L) |
y: peak area (AU\5min); x: mass concentration of analytes, mg/L. LOD: calculated on the basis of 3s/k (s: the deviation of baseline; k: the slope of the linear equation). LOQ: calculated on the basis of 10s/k. | ||||||
2-NP | 21514 | 10-500 | y=4399.46x+10176.18 | 0.9977 | 0.13 | 0.45 |
4-NP | 20529 | 10-500 | y=2575.18x+25294.24 | 0.9998 | 0.23 | 0.76 |
DNP | 17352 | 20-1000 | y=2881.43x+71.93 | 0.9975 | 0.20 | 0.68 |
TNP | 11262 | 20-1000 | y=3283.97x+6775.26 | 0.9959 | 0.18 | 0.60 |
Analyte | Intra-day (n=3) | Inter-day (n=3) | Column-to-column (n=3) | |||||
Migration time | Peak area | Migration time | Peak area | Migration time | Peak area | |||
2-NP | 1.4 | 1.6 | 5.7 | 7.0 | 3.6 | 3.5 | ||
4-NP | 1.5 | 1.6 | 6.4 | 5.6 | 3.7 | 7.6 | ||
DNP | 1.4 | 1.2 | 5.9 | 2.5 | 5.5 | 5.8 | ||
TNP | 1.4 | 0.6 | 6.8 | 4.3 | 4.5 | 9.4 |
Table 2 Intra-day, inter-day and column-to-column RSDs of the migration time and peak areas for the four nitrophenol analytes %
Analyte | Intra-day (n=3) | Inter-day (n=3) | Column-to-column (n=3) | |||||
Migration time | Peak area | Migration time | Peak area | Migration time | Peak area | |||
2-NP | 1.4 | 1.6 | 5.7 | 7.0 | 3.6 | 3.5 | ||
4-NP | 1.5 | 1.6 | 6.4 | 5.6 | 3.7 | 7.6 | ||
DNP | 1.4 | 1.2 | 5.9 | 2.5 | 5.5 | 5.8 | ||
TNP | 1.4 | 0.6 | 6.8 | 4.3 | 4.5 | 9.4 |
Analyte | Chemical structure | log Kowa | Molecule sizeb/nm | Molecular volumec/nm3 |
a) log Kow came from SciFinder. b) The molecular size calculated with Accelrys Discover Studio Client. c) The molecular volume calculated with HyperChem. | ||||
2-NP | 1.671 | 0.528-0.605 | 0.409 | |
4-NP | 1.668 | 0.428-0.681 | 0.422 | |
DNP | 1.715 | 0.567-0.681 | 0.471 | |
TNP | 1.679 | 0.617-0.701 | 0.521 |
Table 3 Chemical structures, log Kow, molecular sizes and molecular volumes of the four nitrophenol analytes
Analyte | Chemical structure | log Kowa | Molecule sizeb/nm | Molecular volumec/nm3 |
a) log Kow came from SciFinder. b) The molecular size calculated with Accelrys Discover Studio Client. c) The molecular volume calculated with HyperChem. | ||||
2-NP | 1.671 | 0.528-0.605 | 0.409 | |
4-NP | 1.668 | 0.428-0.681 | 0.422 | |
DNP | 1.715 | 0.567-0.681 | 0.471 | |
TNP | 1.679 | 0.617-0.701 | 0.521 |
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