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Quantitative Analysis of Fentanyl and Six Fentanyl Analogs in Postmortem Specimens by UHPLC-MS-MS.
J Anal Toxicol. 2018 Oct 01; 42(8):570-580.JA

Abstract

Since 2013, opioid-related deaths have increased in Miami-Dade County, FL due to fentanyl and fentanyl analogs in the local heroin supply. From 2014 to 2015, a near 600% increase in fentanyl and fentanyl analog-related deaths was observed, followed by another 200% increase in 2016. In addition to fentanyl, six fentanyl analogs were identified in this time period: β-hydroxythiofentanyl, acetyl fentanyl, furanyl fentanyl, carfentanil, butyryl fentanyl and para-fluoroisobutyryl fentanyl. As a result, an analytical method to quantify these compounds in postmortem biological fluids and tissues using solid-phase extraction with analysis by ultra high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS-MS) was developed and validated. All analytes except carfentanil were linear from 1 to 50 ng/mL with a limit of detection (LOD) of 0.5 ng/mL; carfentanil was linear from 0.2 to 10 ng/mL with a LOD of 0.1 ng/mL. For all analytes, bias was within ±14%, intra- and inter-day precision were ≤5% and extraction efficiency was >87%. Dilution integrity was assessed at 1:1, 1:4 and 1:9 (v/v) ratios; percent error from target was <12% for all analytes. No exogenous interferences were observed. Analytes were stable in preserved whole blood stored at 4°C for 9 months; extracted samples were stable in the refrigerated autosampler (15°C) for up to 72 h. The ability to distinguish the isomer pairs isobutyryl/butyryl fentanyl and p-fluoroisobutyryl/p-fluorobutyryl fentanyl is achieved by this method. The method was applied to 312 cases in which fentanyl and/or fentanyl analogs were previously identified. Postmortem concentrations in blood ranged from <0.2 to 0.73 ng/mL for carfentanil and from 30.6 to 91.7 ng/mL for p-fluoroisobutyryl fentanyl in cases in which these analytes were listed as the sole cause of death.

Authors+Show Affiliations

Miami-Dade Medical Examiner Department, 1851 NW 10th Avenue, Miami, FL, USA.Miami-Dade Medical Examiner Department, 1851 NW 10th Avenue, Miami, FL, USA.Miami-Dade Medical Examiner Department, 1851 NW 10th Avenue, Miami, FL, USA.Miami-Dade Medical Examiner Department, 1851 NW 10th Avenue, Miami, FL, USA.Miami-Dade Medical Examiner Department, 1851 NW 10th Avenue, Miami, FL, USA.

Pub Type(s)

Journal Article

Language

eng

PubMed ID

30371841

Citation

Kahl, Joseph H., et al. "Quantitative Analysis of Fentanyl and Six Fentanyl Analogs in Postmortem Specimens By UHPLC-MS-MS." Journal of Analytical Toxicology, vol. 42, no. 8, 2018, pp. 570-580.
Kahl JH, Gonyea J, Humphrey SM, et al. Quantitative Analysis of Fentanyl and Six Fentanyl Analogs in Postmortem Specimens by UHPLC-MS-MS. J Anal Toxicol. 2018;42(8):570-580.
Kahl, J. H., Gonyea, J., Humphrey, S. M., Hime, G. W., & Boland, D. M. (2018). Quantitative Analysis of Fentanyl and Six Fentanyl Analogs in Postmortem Specimens by UHPLC-MS-MS. Journal of Analytical Toxicology, 42(8), 570-580. https://doi.org/10.1093/jat/bky054
Kahl JH, et al. Quantitative Analysis of Fentanyl and Six Fentanyl Analogs in Postmortem Specimens By UHPLC-MS-MS. J Anal Toxicol. 2018 Oct 1;42(8):570-580. PubMed PMID: 30371841.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Quantitative Analysis of Fentanyl and Six Fentanyl Analogs in Postmortem Specimens by UHPLC-MS-MS. AU - Kahl,Joseph H, AU - Gonyea,Jennifer, AU - Humphrey,Susan M, AU - Hime,George W, AU - Boland,Diane M, PY - 2018/03/13/received PY - 2018/07/16/accepted PY - 2018/10/30/entrez PY - 2018/10/30/pubmed PY - 2019/1/12/medline SP - 570 EP - 580 JF - Journal of analytical toxicology JO - J Anal Toxicol VL - 42 IS - 8 N2 - Since 2013, opioid-related deaths have increased in Miami-Dade County, FL due to fentanyl and fentanyl analogs in the local heroin supply. From 2014 to 2015, a near 600% increase in fentanyl and fentanyl analog-related deaths was observed, followed by another 200% increase in 2016. In addition to fentanyl, six fentanyl analogs were identified in this time period: β-hydroxythiofentanyl, acetyl fentanyl, furanyl fentanyl, carfentanil, butyryl fentanyl and para-fluoroisobutyryl fentanyl. As a result, an analytical method to quantify these compounds in postmortem biological fluids and tissues using solid-phase extraction with analysis by ultra high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS-MS) was developed and validated. All analytes except carfentanil were linear from 1 to 50 ng/mL with a limit of detection (LOD) of 0.5 ng/mL; carfentanil was linear from 0.2 to 10 ng/mL with a LOD of 0.1 ng/mL. For all analytes, bias was within ±14%, intra- and inter-day precision were ≤5% and extraction efficiency was >87%. Dilution integrity was assessed at 1:1, 1:4 and 1:9 (v/v) ratios; percent error from target was <12% for all analytes. No exogenous interferences were observed. Analytes were stable in preserved whole blood stored at 4°C for 9 months; extracted samples were stable in the refrigerated autosampler (15°C) for up to 72 h. The ability to distinguish the isomer pairs isobutyryl/butyryl fentanyl and p-fluoroisobutyryl/p-fluorobutyryl fentanyl is achieved by this method. The method was applied to 312 cases in which fentanyl and/or fentanyl analogs were previously identified. Postmortem concentrations in blood ranged from <0.2 to 0.73 ng/mL for carfentanil and from 30.6 to 91.7 ng/mL for p-fluoroisobutyryl fentanyl in cases in which these analytes were listed as the sole cause of death. SN - 1945-2403 UR - https://www.unboundmedicine.com/medline/citation/30371841/Quantitative_Analysis_of_Fentanyl_and_Six_Fentanyl_Analogs_in_Postmortem_Specimens_by_UHPLC_MS_MS_ L2 - https://academic.oup.com/jat/article-lookup/doi/10.1093/jat/bky054 DB - PRIME DP - Unbound Medicine ER -