Chinese Journal of Chromatography ›› 2023, Vol. 41 ›› Issue (7): 572-581.DOI: 10.3724/SP.J.1123.2022.09004
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ZHAO Yuanqing1, HU Kai1,*(), YANG Cheng1, HAN Pengzhao1, LI Lixin1, LIU Xiaobing1, ZHANG Zhenqiang1, ZHANG Shusheng2
Received:
2022-09-05
Online:
2023-07-08
Published:
2023-06-30
Supported by:
CLC Number:
ZHAO Yuanqing, HU Kai, YANG Cheng, HAN Pengzhao, LI Lixin, LIU Xiaobing, ZHANG Zhenqiang, ZHANG Shusheng. Determination of catecholamines in urine by disperse solid-phase extraction-liquid chromatography based on Ti3C2Tx/polyimide composites[J]. Chinese Journal of Chromatography, 2023, 41(7): 572-581.
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URL: https://www.chrom-china.com/EN/10.3724/SP.J.1123.2022.09004
Fig. 1 Preparation process of composites (Ti3C2Tx/PI) and sample extraction process Ti3C2Tx: two dimensional titanium carbide; PI: polyimide: CAs: catecholamines; APTES: 3-aminopropyltriethoxysilane.
Fig. 2 (a, b) SEM images and (c, d, e, f) energy dispersive spectra (EDS) of Ti3C2Tx/PI a. magnification, 20000; b. magnification,10000; c. C; d. N; e. O; f. Ti.
Fig. 4 Effects of (a) adsorption time, (b) sample pH, (c) adsorbent dosage, (d) desorption solvent, (e) desorption time on the recoveries of the targets (n=3) NE: noradrenaline; E: adrenaline; DA: dopamine; ISO: isoproterenol; HAc: acetic acid. Desorption solvents: 1. MeOH; 2. ACN; 3. 5%(v/v) HAc-MeOH 4. 5%(v/v) HAc-ACN; 5. HAc-MeOH-H2O (5∶47.5∶47.5, v/v/v); 6. HAc-ACN-H2O (5∶47.5∶47.5, v/v/v).
Analyte | Linear equation | r2 | Linear range/ (ng/mL) | LOD/ (ng/mL) | LOQ/ (ng/mL) | RSDs/% | |
---|---|---|---|---|---|---|---|
Intra-day (n=6) | Inter-day (n=3) | ||||||
NE | y=5.68×10-2x-1.96×10-2 | 0.9982 | 1.0-250 | 0.32 | 1.0 | 1.09 | 4.24 |
E | y=5.14×10-2x-3.48×10-2 | 0.9962 | 1.0-250 | 0.30 | 1.0 | 0.57 | 1.73 |
DA | y=5.36×10-2x+3.72×10-2 | 0.9977 | 1.0-250 | 0.20 | 0.7 | 0.80 | 2.64 |
ISO | y=5.75×10-2x-2.04×10-2 | 0.9931 | 1.0-250 | 0.30 | 1.0 | 0.59 | 2.73 |
Table 1 Linear equations, correlation coefficients (r2), linear ranges, limits of detection (LODs), limits of quantification (LOQs) and relative standard deviations (RSDs) of the four CAs
Analyte | Linear equation | r2 | Linear range/ (ng/mL) | LOD/ (ng/mL) | LOQ/ (ng/mL) | RSDs/% | |
---|---|---|---|---|---|---|---|
Intra-day (n=6) | Inter-day (n=3) | ||||||
NE | y=5.68×10-2x-1.96×10-2 | 0.9982 | 1.0-250 | 0.32 | 1.0 | 1.09 | 4.24 |
E | y=5.14×10-2x-3.48×10-2 | 0.9962 | 1.0-250 | 0.30 | 1.0 | 0.57 | 1.73 |
DA | y=5.36×10-2x+3.72×10-2 | 0.9977 | 1.0-250 | 0.20 | 0.7 | 0.80 | 2.64 |
ISO | y=5.75×10-2x-2.04×10-2 | 0.9931 | 1.0-250 | 0.30 | 1.0 | 0.59 | 2.73 |
Analyte | Smoker | Non-smoker | |||||
---|---|---|---|---|---|---|---|
Sample 1 | Sample 2 | Sample 3 | Sample 1 | Sample 2 | Sample 3 | ||
NE | 9.05 | 9.22 | 13.26 | 2.00 | 1.47 | 1.65 | |
E | 10.22 | 4.65 | 9.18 | 1.95 | 2.91 | 2.65 | |
DA | 21.58 | 15.8 | 11.32 | 6.27 | 7.40 | 4.98 | |
ISO | ND | ND | ND | ND | ND | ND |
Table 2 Contents of CAs in urine samples of smokers and non-smokers ng/mL
Analyte | Smoker | Non-smoker | |||||
---|---|---|---|---|---|---|---|
Sample 1 | Sample 2 | Sample 3 | Sample 1 | Sample 2 | Sample 3 | ||
NE | 9.05 | 9.22 | 13.26 | 2.00 | 1.47 | 1.65 | |
E | 10.22 | 4.65 | 9.18 | 1.95 | 2.91 | 2.65 | |
DA | 21.58 | 15.8 | 11.32 | 6.27 | 7.40 | 4.98 | |
ISO | ND | ND | ND | ND | ND | ND |
Analyte | 25 ng/mL | 100 ng/mL | 250 ng/mL | |||||
---|---|---|---|---|---|---|---|---|
Recovery/% | RSD/% | Recovery/% | RSD/% | Recovery/% | RSD/% | |||
NE | 93.31 | 9.23 | 82.50 | 2.47 | 93.25 | 2.99 | ||
E | 96.25 | 5.53 | 83.57 | 3.16 | 92.67 | 5.65 | ||
DA | 87.38 | 8.07 | 94.86 | 4.16 | 96.85 | 5.07 | ||
ISO | 89.15 | 9.96 | 92.44 | 6.04 | 83.64 | 2.63 |
Table 3 Recoveries and precisions of the four CAs in urine samples at three spiked levels (n=3)
Analyte | 25 ng/mL | 100 ng/mL | 250 ng/mL | |||||
---|---|---|---|---|---|---|---|---|
Recovery/% | RSD/% | Recovery/% | RSD/% | Recovery/% | RSD/% | |||
NE | 93.31 | 9.23 | 82.50 | 2.47 | 93.25 | 2.99 | ||
E | 96.25 | 5.53 | 83.57 | 3.16 | 92.67 | 5.65 | ||
DA | 87.38 | 8.07 | 94.86 | 4.16 | 96.85 | 5.07 | ||
ISO | 89.15 | 9.96 | 92.44 | 6.04 | 83.64 | 2.63 |
Detection system | Materials | Extraction/ min | Linear range/ (ng/mL) | LODs/ (ng/mL) | Recoveries/ % | RSDs/ % | Ref. |
---|---|---|---|---|---|---|---|
HPLC-FLD | magGO@POSS-BA | 2 | 10-500 | 0.54-2.28 | 81.3-101.7 | 6.9-9.7 | [ |
HPLC-FLD | Fe3O4@SiO2/IDA-Cu | 30 | 0.7-50 | 0.20-0.33 | 86.2-109.4 | 3.8-10.0 | [ |
HPLC-UV | BA-RAM | 30 | 5-100 | - | 87-114 | 7.6-14.4 | [ |
LC-MS/MS | ZrO2 | 10 | 1-200 | 0.035-0.050 | 91.0-109.5 | 2.8-9.4 | [ |
HPLC-FLD | Fe3O4@COF@2-FPBA | 60 | 2-200 | 0.31-0.54 | 86.3-114.9 | 2.34-10.5 | [ |
HPLC-FLD | Fe3O4@Ti3C2Tx-BA | 2 | 1-500 | 0.03-0.16 | 88.14-112.3 | 3.03-11.7 | [ |
HPLC-FLD | Ti3C2Tx/PI | 10 | 1-250 | 0.20-0.32 | 82.50-96.85 | 2.47-9.96 | this work |
Table 4 Comparison of the method with other methods in references
Detection system | Materials | Extraction/ min | Linear range/ (ng/mL) | LODs/ (ng/mL) | Recoveries/ % | RSDs/ % | Ref. |
---|---|---|---|---|---|---|---|
HPLC-FLD | magGO@POSS-BA | 2 | 10-500 | 0.54-2.28 | 81.3-101.7 | 6.9-9.7 | [ |
HPLC-FLD | Fe3O4@SiO2/IDA-Cu | 30 | 0.7-50 | 0.20-0.33 | 86.2-109.4 | 3.8-10.0 | [ |
HPLC-UV | BA-RAM | 30 | 5-100 | - | 87-114 | 7.6-14.4 | [ |
LC-MS/MS | ZrO2 | 10 | 1-200 | 0.035-0.050 | 91.0-109.5 | 2.8-9.4 | [ |
HPLC-FLD | Fe3O4@COF@2-FPBA | 60 | 2-200 | 0.31-0.54 | 86.3-114.9 | 2.34-10.5 | [ |
HPLC-FLD | Fe3O4@Ti3C2Tx-BA | 2 | 1-500 | 0.03-0.16 | 88.14-112.3 | 3.03-11.7 | [ |
HPLC-FLD | Ti3C2Tx/PI | 10 | 1-250 | 0.20-0.32 | 82.50-96.85 | 2.47-9.96 | this work |
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