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| Content Provider | World Health Organization (WHO)-Global Index Medicus |
|---|---|
| Author | Verplaetse, Ruth Tytgat, Jan |
| Description | Country affiliation: Belgium Author Affiliation: Verplaetse R ( Laboratory of Toxicology, KULeuven, Campus Gasthuisberg O&N 2, PO Box 922, Herestraat 49, 3000 Leuven, Belgium. ruth.verplaetse@pharm.kuleuven.be) |
| Abstract | Fentanyl and its major metabolite norfentanyl often occur in low doses in biological samples. Therefore, a highly sensitive liquid chromatography tandem mass spectrometry (LC-MS/MS) method has been developed and fully validated. Sample preparation was performed on a mixed-mode cation exchange solid phase extraction (SPE) cartridge with an additional alkaline wash step to decrease matrix effects and thus increase sensitivity. Ionization of fentanyl and norfentanyl with electrospray ionization (ESI) was more efficient than atmospheric pressure chemical ionization (APCI). The use of a mobile phase of high pH resulted in higher ESI signals than the conventional low pH mobile phases. In the final method, gradient elution with 10 mM ammonium bicarbonate (pH 9) and methanol was performed. A comparison of columns with different internal diameter and/or smaller particles showed optimal resolution and sensitivity when an Acquity C18 column (1.7 microm, 2.1 mm x 50 mm) was used. Deuterium labeled internal standards were used, but with careful evaluation of their stability since loss of deuteriums was seen. With limits of detection of 0.25 pg/ml for fentanyl and 2.5 pg/ml for norfentanyl in urine and 5 pg/ml for fentanyl and norfentanyl in whole blood the presented method is highly appropriate for the analysis of fentanyl and norfentanyl in forensic urine and blood samples. |
| File Format | HTM / HTML |
| ISSN | 15700232 |
| Issue Number | 22 |
| Volume Number | 878 |
| e-ISSN | 1873376X |
| Journal | Journal of Chromatography B |
| Language | English |
| Publisher | Elsevier |
| Publisher Date | 2010-07-15 |
| Publisher Place | Netherlands |
| Access Restriction | One Nation One Subscription (ONOS) |
| Subject Keyword | Discipline Analytical Chemistry Chromatography, High Pressure Liquid Methods Fentanyl Analogs & Derivatives Blood Urine Tandem Mass Spectrometry Metabolism Forensic Sciences Humans Evaluation Studies Journal Article Validation Studies |
| Content Type | Text |
| Resource Type | Article |
| Subject | Cell Biology Medicine Analytical Chemistry Clinical Biochemistry Biochemistry |
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