Efficient Sub-1 Minute Analysis of Selected Biomarker Catecholamines by Core-Shell Hydrophilic Interaction Liquid Chromatography (HILIC) with Nanomolar Detection at a Boron-Doped Diamond (BDD) Electrode
Abstract
:1. Introduction
2. Materials and Methods
2.1. Chemicals and Materials
2.2. Cyclic Voltammetry (CV)
2.3. HPLC Instrumentation
2.4. Chromatographic Conditions
2.5. Validation Procedures
3. Results and Discussion
3.1. Electrochemical Behavior of the CAs Using Cyclic Voltammetry (CV)
3.2. Comparison of Zwitterionic HILIC Columns
3.3. Optimization of HILIC Separation Conditions
3.4. Optimization of Detection Potential for LC-ECD
3.5. Method Validation
3.6. Urine Sample Analysis
4. Conclusions
Supplementary Materials
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Acknowledgments
Conflicts of Interest
References
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HILIC Columns | Analyte | N/m | RSD (%) |
---|---|---|---|
Poro-Shell Z-HILIC | DA | 49,040 | 0.98 |
EPI | 43,132 | 0.91 | |
NE | 44,172 | 1.86 | |
Fully Porous Z-cHILIC | DA | 23,019 | 0.72 |
EPI | 23,887 | 1.04 | |
NE | 31,247 | 1.36 | |
Fully Porous Z-HILIC | DA | 18,395 | 0.69 |
EPI | 16,973 | 2.01 | |
NE | 22,598 | 2.27 |
HILIC Columns | Analyte | α | RSD (%) |
---|---|---|---|
Poro-Shell Z-HILIC | DA& EPI | 1.30 | 0.572 |
EPI& NE | 1.39 | 0.187 | |
Fully Porous Z-cHILIC | DA& EPI | 1.22 | 0.417 |
EPI& NE | 1.84 | 0.132 | |
Fully Porous Z-HILIC | DA& EPI | 1.26 | 0.231 |
EPI& NE | 1.71 | 0.214 |
Analyte | Linear Range (µM) | Linear Regression Equation | Correlation Coefficient (R2) | LOD a HPLC-ECD (nM) | LOD b HPLC-UV (µM) |
---|---|---|---|---|---|
DA | 0.1–25 | y = 6 × 10−8 C − 4 × 10−9 | 0.994 | 40 | 0.5 |
EPI | 0.1–25 | y = 5 × 10−8 C − 3 × 10−9 | 0.993 | 50 | 0.7 |
NE | 0.1–25 | y = 4 × 10−8 C − 4 × 10−9 | 0.995 | 50 | 1 |
Technique | Analytes | Separation Time | LOD | Ref. |
---|---|---|---|---|
CE-CL | DA EPI NE | 6 min | 69 nM 79 nM 100 nM | [62] |
MMIP-CE | DA EPI NE | 8 min | 60 nM 60 nM 50 nM | [63] |
HPLC- fluorescence detection | DA EPI NE | 40 min | 0.1 nM 0.4 nM 0.4 nM | [29] |
RP-Amperometric detection (BDD electrode) | DA EPI NE | 9 min | 4 × 10−3 µg/mL (26 nM) 2 × 10−3 µg/mL (11 nM) 4 × 10−3 µg/mL (23 nM) | [65] |
HPLC-MS-MS | DA EPI NE | 6 min | 5 nM 10 nM 10 nM | [64] |
HILIC- Amperometric detection (BDD electrode) | DA EPI NE | less than 1 min | 40 nM (7.5 × 10−3 µg/mL) 50 nM (10.6 × 10−3 µg/mL) 50 nM (10.2 × 10−3 µg/mL) | This work |
Analyte | RSD a (%) Intra-Day | RSD b (%) Inter-Day |
---|---|---|
DA | 0.42 | 0.65 |
EPI | 0.35 | 0.40 |
NE | 0.36 | 0.49 |
Analytes | Concentration (nM) in Unspiked Urine | Concentration (nM) Added | Concentration (nM) Found | Recovery % | RSD % |
---|---|---|---|---|---|
DA | 1440 | 600 1500 3000 | 1990 2800 4170 | 91.6 93 90.9 | 4.6 2.7 2.3 |
EPI | ND a | 250 500 1000 | 231 471 915 | 92.4 94 91.5 | 2.3 6 4 |
NE | 112 | 400 800 1600 | 473 840 1550 | 90.3 91 90 | 1.4 2.7 2.4 |
Sample | DA (nM) ± SD | EPI (nM) ± SD | NE (nM) ± SD |
---|---|---|---|
1 | 1440 ± 1.44 | ND a | 112 ± 1.67 |
2 | 1793 ± 1.34 | ND a | 158 ± 2.67 |
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Alsaeedi, M.; Alghamdi, H.; Hayes, P.E.; Hogan, A.M.; Glennon, J.D. Efficient Sub-1 Minute Analysis of Selected Biomarker Catecholamines by Core-Shell Hydrophilic Interaction Liquid Chromatography (HILIC) with Nanomolar Detection at a Boron-Doped Diamond (BDD) Electrode. Separations 2021, 8, 124. https://doi.org/10.3390/separations8080124
Alsaeedi M, Alghamdi H, Hayes PE, Hogan AM, Glennon JD. Efficient Sub-1 Minute Analysis of Selected Biomarker Catecholamines by Core-Shell Hydrophilic Interaction Liquid Chromatography (HILIC) with Nanomolar Detection at a Boron-Doped Diamond (BDD) Electrode. Separations. 2021; 8(8):124. https://doi.org/10.3390/separations8080124
Chicago/Turabian StyleAlsaeedi, Majidah, Huda Alghamdi, Phyllis E. Hayes, Anna M. Hogan, and Jeremy D. Glennon. 2021. "Efficient Sub-1 Minute Analysis of Selected Biomarker Catecholamines by Core-Shell Hydrophilic Interaction Liquid Chromatography (HILIC) with Nanomolar Detection at a Boron-Doped Diamond (BDD) Electrode" Separations 8, no. 8: 124. https://doi.org/10.3390/separations8080124