Miniaturized extraction method for analysis of synthetic opioids in urine by microextraction with packed sorbent and liquid chromatography-tandem mass spectrometry

Author(s)

da Cunha, Kelly Francisco ^{[1, 2]} ; Rodrigues, Leonardo Costalonga ^{[3, 2, 4]} ; Huestis, Marilyn A. ^[5] ; Costa, Jose Luiz ^{[3, 2, 4]}

Affiliation

^[1] Univ Estadual Campinas, Fac Med Sci, BR-13083859 Campinas, SP - Brazil

^[2] Univ Estadual Campinas, Fac Med Sci, Campinas Poison Control Ctr, BR-13083859 Campinas, SP - Brazil

^[3] Univ Estadual Campinas, Fac Pharmaceut Sci, BR-13083859 Campinas, SP - Brazil

^[4] Huestis, Marilyn A., Thomas Jefferson Univ, Inst Emerging Hlth Profess, Philadelphia, PA 19107 USA.da Cunha, Kelly Francisco, Univ Estadual Campinas, Fac Med Sci, Campinas Poison Control Ctr, BR-13083859 Campinas, SP - Brazil

^[5] Thomas Jefferson Univ, Inst Emerging Hlth Profess, Philadelphia, PA 19107 - USA

• Document type: Journal article
• Source: Journal of Chromatography A; v. 1624, AUG 2 2020.
• Web of Science Citations: 1

Abstract

Synthetic opioids are responsible for numerous overdoses and fatalities worldwide. Currently, fentanyl and its analogs are also mixed with heroin, cocaine and methamphetamine, or sold as oxycodone, hydrocodone and alprazolam in counterfeit medications. Microextraction techniques became more frequent in analytical toxicology over the last decade. A method to simultaneously quantify nine synthetic opioids, fentanyl, sufentanil, alfentanil, acrylfentanyl, thiofentanyl, valerylfentanyl, furanylfentanyl, acetyl fentanyl and carfentanil, and two metabolites, norfentanyl and acetyl norfentanyl, in urine samples by microextraction with packed sorbent (MEPS) and liquid chromatography-tandem mass spectrometry (LCMS/MS) was developed and validated. A multivariate optimization was performed to establish the number and speed (stroke) of draw-eject sample cycles and the extraction solvent. The best extraction condition was eight draw-eject sample cycles, with a velocity of 3.6 mu L/sec and acetonitrile as elution solvent. Linearity was achieved between 1 to 100 ng/mL, with a limit of detection (LOD) of 0.1 ng/mL and limit of quantification (LOQ) of 1 ng/mL. Imprecision (% relative standard deviation) and bias (%) were less than 12.8% and 5.7%, respectively. The method had good specificity and selectivity when challenged with 10 different matrix sources and 36 pharmaceuticals and drugs of abuse at concentrations of 100 or 500 ng/mL. The method was successfully applied to authentic urine samples. MEPS was an efficient semi-automatic extraction technique, requiring small volumes of organic solvents (640 mu L) and sample (200 mu L). The cartridges can be cleaned and reused (average of 150 sample extractions/barrel inside and needle). (C)2020 Elsevier B.V. All rights reserved. (AU)

• FAPESP's process: 17/02147-0 - Single drop chromatography and its coupling to mass spectrometry: instrumental strategies, development of materials, automation and analytical applications
• Grantee: Fernando Mauro Lanças
• Support Opportunities: Research Projects - Thematic Grants
• FAPESP's process: 18/11849-0 - The toxicology of New Psychoactive Substances (NSP): epidemiology of consumption by oral fluid samples and characterization of their in vitro metabolism
• Grantee: Kelly Francisco da Cunha
• Support Opportunities: Scholarships in Brazil - Doctorate
• FAPESP's process: 17/24515-0 - Development of a microextraction by packed sorbent (MEPS) method to analysis of synthetic opioids in urine samples
• Grantee: Leonardo Costalonga Rodrigues
• Support Opportunities: Scholarships in Brazil - Scientific Initiation
• FAPESP's process: 18/00432-1 - The Toxicology of New Psychoactive Substances (NSP): epidemiology of consumption by the analysis of hair and oral fluid samples
• Grantee: José Luiz da Costa
• Support Opportunities: Regular Research Grants