Determination of Immunosuppressive Drugs by Dispersive Liquid-Liquid Microextraction Combined with Surface-Assisted Laser Desorption/Ionization Mass Spectrometry
| Autor: | Pin-Shiuan Chen, 陳品璇 |
|---|---|
| Rok vydání: | 2014 |
| Druh dokumentu: | 學位論文 ; thesis |
| Popis: | 102 A novel method for the determination of immunosuppressive drugs using dispersive liquid–liquid microextraction (DLLME) coupled to surface-assisted laser desorption/ionization mass spectrometric (SALDI-MS) detection was developed. Acetone and dichloromethane were used as the disperser solvent and extraction solvent, respectively. A mixture of extraction solvent and disperser solvent were rapidly injected into a 1.0 mL aqueous sample to form a cloudy solution. After the extraction, immunosuppressive drugs were detected using surface-assisted laser desorption/ionization mass spectrometry (SALDI/MS) with colloidal Pd and α-CHCA as the co-matrix. Under optimum conditions, the limits of detection (LODs) at a signal-to-noise ratio of 3 were 3, 3, and 14 nM for cyclosporine (CsA), everolimus (ERL), and sirolimus (SRL), respectively. With a sample-to-extract volume ratio of 200, the enrichment factor for immunosuppressive drugs was calculated to be 108, 122 and 101 for CsA, ERL and SRL, respectively. This developed method was successfully applied to the determination of immunosuppressive drugs in human urine samples. The LODs of CsA, ERL and SRL in human urine sample were 6, 6 and 29 nM, respectively. Recoveries of CsA、ERL and SRL were calculated to be 53.8%, 61.0% and 50.7%, respectively. The precision and accuracy of the Intra-day and Inter-day were less than 10% (n = 5). DLLME technique is simple, rapid and cheap. DLLME combined SALDI-MS method offers high extraction efficiency, low limit of detection and eco-friendly, etc. |
| Databáze: | Networked Digital Library of Theses & Dissertations |
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