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Quantitative Online Liquid Chromatography-Surface-Enhanced Raman Scattering (LC-SERS) of Methotrexate and its Major Metabolites
- Source :
- Subaihi, A, Trivedi, D, Hollywood, K, Bluett, J, Xu, Y, Muhamad Ali, H, Ellis, D & Goodacre, R 2017, ' Quantitative, Liquid Chromatography-Surface-Enhanced Raman Scattering (LC-SERS) of Methotrexate and its Major Metabolites ', Analytical Chemistry, vol. 89, no. 12, pp. 6702-6709 . https://doi.org/10.1021/acs.analchem.7b00916
- Publication Year :
- 2017
-
Abstract
- The application of Raman spectroscopy as a detection method coupled with liquid chromatography (LC) has recently attracted considerable interest, although this has currently been limited to isocratic elution. The combination of LC with rapidly advancing Raman techniques, such as surface-enhanced Raman scattering (SERS), allows for rapid separation, identification and quantification, leading to quantitative discrimination of closely eluting analytes. This study has demonstrated the utility of SERS in conjunction with reversed-phase liquid chromatography (RP-LC), for the detection and quantification of the therapeutically relevant drug molecule methotrexate (MTX) and its metabolites 7-hydroxy methotrexate (7-OH MTX) and 2,4-diamino-N(10)-methylpteroic acid (DAMPA) in pure solutions and mixtures, including spikes into human urine from a healthy individual and patients under medication. While the RP-LC analysis developed employed gradient elution, where the chemical constituents of the mobile phase were modified stepwise during analysis, this did not overtly interfere with the SERS signals. In addition, the practicability and clinical utility of this approach has also been demonstrated using authentic patients' urine samples. Here, the identification of MTX, 7-OH MTX and DAMPA are based on their unique SERS spectra, providing limits of detection of 2.36, 1.84, and 3.26 μM respectively. Although these analytes are amenable to LC and LC-MS detection an additional major benefit of the SERS approach is its applicability toward the detection of analytes that do not show UV absorption or are not ionised for mass spectrometry (MS)-based detection. The results of this study clearly demonstrate the potential application of online LC-SERS analysis for real-time high-throughput detection of drugs and their related metabolites in human biofluids.
- Subjects :
- Analyte
Surface Properties
LC
Liquid chromatography
02 engineering and technology
Urine
Spectrum Analysis, Raman
01 natural sciences
Analytical Chemistry
symbols.namesake
Metabolomics
Manchester Institute of Biotechnology
Autoimmune disease
medicine
Molecule
Rheumatoid arthiritis
Humans
Raman
Cancer
Chromatography
Isocratic elution
Neoplasia
Molecular Structure
Chemistry
SERS
010401 analytical chemistry
021001 nanoscience & nanotechnology
ResearchInstitutes_Networks_Beacons/manchester_institute_of_biotechnology
0104 chemical sciences
Methotrexate
symbols
Gradient elution
0210 nano-technology
Raman spectroscopy
Raman scattering
medicine.drug
Chromatography, Liquid
Subjects
Details
- ISSN :
- 15206882
- Volume :
- 89
- Issue :
- 12
- Database :
- OpenAIRE
- Journal :
- Analytical chemistry
- Accession number :
- edsair.doi.dedup.....de3d51528cae9495b10e7e2ac8850edb