Highly sensitive gas chromatographic—mass spectrometric screening method for the determination of picogram levels of fentanyl, sufentanil and alfentanil and their major metabolites in urine of o
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- 作者：Van Nimmen ; Nadine F.J. ; Poels ; Katrien L.C. ; Veulemans ; Hendrik A.F.
- 关键词：Occupational exposure ; Fentanyl ; Sufentanil ; Alfentanil
- 刊名：Journal of Chromatography B, Analytical Technologies in the Biomedical and Life Sciences
- 出版年：2004
- 出版时间：May 25, 2004
- 年：2004
- 卷：804
- 期：2
- 页码：375-387
- 全文大小：200 K
文摘
Highly sensitive and specific analytical GC–MS procedures were developed and comprehensively validated for the determination of the opioid narcotics fentanyl, sufentanil and alfentanil and their major nor-metabolites in urine of potentially exposed opioid production workers. A simple, one step extraction protocol was developed using commercially available solid phase extraction (SPE) columns to recover all analytes from urine. The secondary amine functionalities of the nor-metabolites were derivatized to form stable, pentafluorobenzamide (PFBA)-derivatives with good chromatographic properties. Using the penta-deuterated analogues as internal standards, a limit-of-detection (LOD) of 2.5pg fentanyl/ml, 2.5pg sufentanil/ml and 7.5pg alfentanil/ml urine was achieved. For the opioid metabolites the LODs were found to be <50pg/ml urine. The developed analytical procedures show excellent intra-assay accuracy, particularly considering the ultra low levels of the analytes, with relative errors generally below 10 % . Overall, an excellent reproducibility was observed with coefficients of variation below 10 % at all spike levels for all opioid parent compounds and their metabolites, except for low norfentanyl concentrations. Upon storage at −30°C urine samples were found to be stable for at least 2 months as no significant losses of either compound were observed. The developed analytical procedures have been successfully applied in a biological monitoring survey of fentanyl exposed production workers.