A rapid MCM-41 dispersive micro-solid phase extraction coupled with LC/MS/MS for quantification of ketoconazole and voriconazole in biological fluids
A rapid dispersive micro-solid phase extraction (D-μ-SPE) combined with LC/MS/MS method was developed and validated for the determination of ketoconazole and voriconazole in human urine and plasma samples. Synthesized mesoporous silica MCM-41 was used as sorbent in d-μ-SPE of the azole compounds fro...
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| Format: | Article |
| Language: | English |
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John Wiley & Sons
2017
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| Online Access: | http://psasir.upm.edu.my/id/eprint/59672/ http://psasir.upm.edu.my/id/eprint/59672/1/A%20rapid%20MCM-41%20dispersive%20micro-solid%20phase.pdf |
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| author | Yahaya, Noorfatimah Sanagi, Mohd Marsin Abd Aziz, Noorizan Wan Ibrahim, Wan Aini Nur, Hadi Loh, Saw Hong Kamaruzaman, Sazlinda |
| author_facet | Yahaya, Noorfatimah Sanagi, Mohd Marsin Abd Aziz, Noorizan Wan Ibrahim, Wan Aini Nur, Hadi Loh, Saw Hong Kamaruzaman, Sazlinda |
| author_sort | Yahaya, Noorfatimah |
| building | UPM Institutional Repository |
| collection | Online Access |
| description | A rapid dispersive micro-solid phase extraction (D-μ-SPE) combined with LC/MS/MS method was developed and validated for the determination of ketoconazole and voriconazole in human urine and plasma samples. Synthesized mesoporous silica MCM-41 was used as sorbent in d-μ-SPE of the azole compounds from biological fluids. Important D-μ-SPE parameters, namely type desorption solvent, extraction time, sample pH, salt addition, desorption time, amount of sorbent and sample volume were optimized. Liquid chromatographic separations were carried out on a Zorbax SB-C18 column (2.1 × 100 mm, 3.5 μm), using a mobile phase of acetonitrile–0.05% formic acid in 5 mm ammonium acetate buffer (70:30, v/v). A triple quadrupole mass spectrometer with positive ionization mode was used for the determination of target analytes. Under the optimized conditions, the calibration curves showed good linearity in the range of 0.1–10,000 μg/L with satisfactory limit of detection (≤0.06 μg/L) and limit of quantitation (≤0.3 μg/L). The proposed method also showed acceptable intra- and inter-day precisions for ketoconazole and voriconazole from urine and human plasma with RSD ≤16.5% and good relative recoveries in the range 84.3–114.8%. The MCM-41-D-μ-SPE method proved to be rapid and simple and requires a small volume of organic solvent (200 μL); thus it is advantageous for routine drug analysis. |
| first_indexed | 2025-11-15T11:02:42Z |
| format | Article |
| id | upm-59672 |
| institution | Universiti Putra Malaysia |
| institution_category | Local University |
| language | English |
| last_indexed | 2025-11-15T11:02:42Z |
| publishDate | 2017 |
| publisher | John Wiley & Sons |
| recordtype | eprints |
| repository_type | Digital Repository |
| spelling | upm-596722018-03-15T08:08:17Z http://psasir.upm.edu.my/id/eprint/59672/ A rapid MCM-41 dispersive micro-solid phase extraction coupled with LC/MS/MS for quantification of ketoconazole and voriconazole in biological fluids Yahaya, Noorfatimah Sanagi, Mohd Marsin Abd Aziz, Noorizan Wan Ibrahim, Wan Aini Nur, Hadi Loh, Saw Hong Kamaruzaman, Sazlinda A rapid dispersive micro-solid phase extraction (D-μ-SPE) combined with LC/MS/MS method was developed and validated for the determination of ketoconazole and voriconazole in human urine and plasma samples. Synthesized mesoporous silica MCM-41 was used as sorbent in d-μ-SPE of the azole compounds from biological fluids. Important D-μ-SPE parameters, namely type desorption solvent, extraction time, sample pH, salt addition, desorption time, amount of sorbent and sample volume were optimized. Liquid chromatographic separations were carried out on a Zorbax SB-C18 column (2.1 × 100 mm, 3.5 μm), using a mobile phase of acetonitrile–0.05% formic acid in 5 mm ammonium acetate buffer (70:30, v/v). A triple quadrupole mass spectrometer with positive ionization mode was used for the determination of target analytes. Under the optimized conditions, the calibration curves showed good linearity in the range of 0.1–10,000 μg/L with satisfactory limit of detection (≤0.06 μg/L) and limit of quantitation (≤0.3 μg/L). The proposed method also showed acceptable intra- and inter-day precisions for ketoconazole and voriconazole from urine and human plasma with RSD ≤16.5% and good relative recoveries in the range 84.3–114.8%. The MCM-41-D-μ-SPE method proved to be rapid and simple and requires a small volume of organic solvent (200 μL); thus it is advantageous for routine drug analysis. John Wiley & Sons 2017 Article PeerReviewed text en http://psasir.upm.edu.my/id/eprint/59672/1/A%20rapid%20MCM-41%20dispersive%20micro-solid%20phase.pdf Yahaya, Noorfatimah and Sanagi, Mohd Marsin and Abd Aziz, Noorizan and Wan Ibrahim, Wan Aini and Nur, Hadi and Loh, Saw Hong and Kamaruzaman, Sazlinda (2017) A rapid MCM-41 dispersive micro-solid phase extraction coupled with LC/MS/MS for quantification of ketoconazole and voriconazole in biological fluids. Biomedical Chromatography, 31 (2). art. no. e3803. pp. 1-8. ISSN 0269-3879; ESSN: 1099-0801 http://onlinelibrary.wiley.com/wol1/doi/10.1002/bmc.3803/abstract 10.1002/bmc.3803 |
| spellingShingle | Yahaya, Noorfatimah Sanagi, Mohd Marsin Abd Aziz, Noorizan Wan Ibrahim, Wan Aini Nur, Hadi Loh, Saw Hong Kamaruzaman, Sazlinda A rapid MCM-41 dispersive micro-solid phase extraction coupled with LC/MS/MS for quantification of ketoconazole and voriconazole in biological fluids |
| title | A rapid MCM-41 dispersive micro-solid phase extraction coupled with LC/MS/MS for quantification of ketoconazole and voriconazole in biological fluids |
| title_full | A rapid MCM-41 dispersive micro-solid phase extraction coupled with LC/MS/MS for quantification of ketoconazole and voriconazole in biological fluids |
| title_fullStr | A rapid MCM-41 dispersive micro-solid phase extraction coupled with LC/MS/MS for quantification of ketoconazole and voriconazole in biological fluids |
| title_full_unstemmed | A rapid MCM-41 dispersive micro-solid phase extraction coupled with LC/MS/MS for quantification of ketoconazole and voriconazole in biological fluids |
| title_short | A rapid MCM-41 dispersive micro-solid phase extraction coupled with LC/MS/MS for quantification of ketoconazole and voriconazole in biological fluids |
| title_sort | rapid mcm-41 dispersive micro-solid phase extraction coupled with lc/ms/ms for quantification of ketoconazole and voriconazole in biological fluids |
| url | http://psasir.upm.edu.my/id/eprint/59672/ http://psasir.upm.edu.my/id/eprint/59672/ http://psasir.upm.edu.my/id/eprint/59672/ http://psasir.upm.edu.my/id/eprint/59672/1/A%20rapid%20MCM-41%20dispersive%20micro-solid%20phase.pdf |