Pipette-tip μSPE coupled with HPLC-MS/MS for trace determination of fluoroquinolones in human urine
A microextraction procedure was developed for the determination of fluoroquinolone (FQ) drugs, namely Ciprofloxacin, Levofloxacin, Lomefloxacin, Moxifloxacin, Norfloxacin and Sparfloxacin, in human urine. The new natural waste-derived material consisting of silica-supported carbon nanoparticle aggre...
| Main Authors: | , , , , |
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| Format: | Article |
| Language: | English |
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Elsevier
2023-12-01
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| Series: | Talanta Open |
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| Online Access: | http://www.sciencedirect.com/science/article/pii/S2666831923000917 |
| _version_ | 1827591014580224000 |
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| author | Francesca Merlo Petra Bianchini Federica Maraschi Andrea Speltini Antonella Profumo |
| author_facet | Francesca Merlo Petra Bianchini Federica Maraschi Andrea Speltini Antonella Profumo |
| author_sort | Francesca Merlo |
| collection | DOAJ |
| description | A microextraction procedure was developed for the determination of fluoroquinolone (FQ) drugs, namely Ciprofloxacin, Levofloxacin, Lomefloxacin, Moxifloxacin, Norfloxacin and Sparfloxacin, in human urine. The new natural waste-derived material consisting of silica-supported carbon nanoparticle aggregates from rice husk ash (nC-RHA@SiO2) was used as sorbent for setting up a straightforward pipette-tip micro-solid-phase extraction (PT-µSPE) prior to HPLC-MS/MS quantification. The analytes were adsorbed on the solid phase (25 mg) through multi-type interactions and, after a washing step (0.1 % v/v formic acid, 5 % v/v ethanol), eluted in alkaline aqueous solution (15 % v/v acetonitrile), thus achieving simultaneous extraction and clean-up. The PT-µSPE coupled with MS2 detection provided satisfactory recovery (67–118 %, n = 3) in 1:1 v/v diluted urine samples (formate buffer, pH 3), good inter-day precision (RSD < 12 %), good matrix-matched linearity in the concentration range 3–80 μg L −1 (R2 > 0.9956), and limited matrix effect. The experimental method quantification limit was 5 µg L −1, suitable for trace determination of such drugs in urine. Compared to the actual microextraction procedures, the PT-µSPE described here is attractive in terms of extraction efficiency, sample throughput, energy consumption, limited use of organic solvents and ease of operation, as evidenced by a greenness evaluation through the AGREEprep software. The final method was applied to FQs determination in blind urine samples. |
| first_indexed | 2024-03-09T01:25:49Z |
| format | Article |
| id | doaj.art-db61abc10b274dd4ba73ab93724d9015 |
| institution | Directory Open Access Journal |
| issn | 2666-8319 |
| language | English |
| last_indexed | 2024-03-09T01:25:49Z |
| publishDate | 2023-12-01 |
| publisher | Elsevier |
| record_format | Article |
| series | Talanta Open |
| spelling | doaj.art-db61abc10b274dd4ba73ab93724d90152023-12-10T06:18:42ZengElsevierTalanta Open2666-83192023-12-018100271Pipette-tip μSPE coupled with HPLC-MS/MS for trace determination of fluoroquinolones in human urineFrancesca Merlo0Petra Bianchini1Federica Maraschi2Andrea Speltini3Antonella Profumo4Department of Chemistry, University of Pavia, 27100 Pavia, ItalyDepartment of Chemistry, University of Pavia, 27100 Pavia, ItalyDepartment of Chemistry, University of Pavia, 27100 Pavia, ItalyCorresponding author.; Department of Chemistry, University of Pavia, 27100 Pavia, ItalyDepartment of Chemistry, University of Pavia, 27100 Pavia, ItalyA microextraction procedure was developed for the determination of fluoroquinolone (FQ) drugs, namely Ciprofloxacin, Levofloxacin, Lomefloxacin, Moxifloxacin, Norfloxacin and Sparfloxacin, in human urine. The new natural waste-derived material consisting of silica-supported carbon nanoparticle aggregates from rice husk ash (nC-RHA@SiO2) was used as sorbent for setting up a straightforward pipette-tip micro-solid-phase extraction (PT-µSPE) prior to HPLC-MS/MS quantification. The analytes were adsorbed on the solid phase (25 mg) through multi-type interactions and, after a washing step (0.1 % v/v formic acid, 5 % v/v ethanol), eluted in alkaline aqueous solution (15 % v/v acetonitrile), thus achieving simultaneous extraction and clean-up. The PT-µSPE coupled with MS2 detection provided satisfactory recovery (67–118 %, n = 3) in 1:1 v/v diluted urine samples (formate buffer, pH 3), good inter-day precision (RSD < 12 %), good matrix-matched linearity in the concentration range 3–80 μg L −1 (R2 > 0.9956), and limited matrix effect. The experimental method quantification limit was 5 µg L −1, suitable for trace determination of such drugs in urine. Compared to the actual microextraction procedures, the PT-µSPE described here is attractive in terms of extraction efficiency, sample throughput, energy consumption, limited use of organic solvents and ease of operation, as evidenced by a greenness evaluation through the AGREEprep software. The final method was applied to FQs determination in blind urine samples.http://www.sciencedirect.com/science/article/pii/S2666831923000917MicroextractionBioanalysisSample preparationExtractionClean-upAntibiotics |
| spellingShingle | Francesca Merlo Petra Bianchini Federica Maraschi Andrea Speltini Antonella Profumo Pipette-tip μSPE coupled with HPLC-MS/MS for trace determination of fluoroquinolones in human urine Talanta Open Microextraction Bioanalysis Sample preparation Extraction Clean-up Antibiotics |
| title | Pipette-tip μSPE coupled with HPLC-MS/MS for trace determination of fluoroquinolones in human urine |
| title_full | Pipette-tip μSPE coupled with HPLC-MS/MS for trace determination of fluoroquinolones in human urine |
| title_fullStr | Pipette-tip μSPE coupled with HPLC-MS/MS for trace determination of fluoroquinolones in human urine |
| title_full_unstemmed | Pipette-tip μSPE coupled with HPLC-MS/MS for trace determination of fluoroquinolones in human urine |
| title_short | Pipette-tip μSPE coupled with HPLC-MS/MS for trace determination of fluoroquinolones in human urine |
| title_sort | pipette tip μspe coupled with hplc ms ms for trace determination of fluoroquinolones in human urine |
| topic | Microextraction Bioanalysis Sample preparation Extraction Clean-up Antibiotics |
| url | http://www.sciencedirect.com/science/article/pii/S2666831923000917 |
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