title: Development, optimization, and validation of a novel extraction procedure for the removal of opiates from human hair's surface.
abstract: Room temperature ionic liquids (ILs) have proved to be efficient extraction media for several systems, and their ability to capture volatile compounds from the atmosphere is well established. We report herein a contactless extraction procedure for the removal of opiate drugs from the surface of human hair. The compounds were chosen as a model drug, particularly due to their low volatility. Equal amounts of IL and hair (about 100 mg) were introduced in a customized Y-shaped vial, and the process occurred simply by heating. After testing several ILs, some of them (e.g. 1-methyl-3-ethanol-imidazolium tetrafluoroborate, phenyl-trimethyl-ammonium triflate or bis(dimethyl) diheptylguanidinium iodide) showed extraction efficiencies higher than 80% for the two studied compounds, morphine and 6-monoacetylmorphine. Using the design of experiments (DOE) approach as an optimization tool, and bearing in mind the hygroscopic properties of the ILs (in particular, 1-methyl-3-ethanol-imidazolium tetrafluoroborate), the process was optimized concerning the following variables: temperature (50-120 ºC), extraction time (8-24 h), IL amount (50-200 mg) and water content of the IL (0.01-60%). This study not only provided the optimum conditions for the process (120 ºC, 16 h, 100 mg of IL containing 40% of water), but has also showed that the water content of the IL represents the variable with the most significant effect on the extraction efficiency. Finally, we validated our method through the comparison of the results obtained by treating hair samples with the described procedure to those obtained using a standard washing method and criteria for positivity.
authors.affiliation: Research Institute for Medicines and Pharmaceutical Sciences (iMed.ULisboa), Faculdade de Farmácia da Universidade de Lisboa, Av. Prof. Gama Pinto, 1649-003, Lisboa, Portugal.|Centro de Química Estrutural do Instituto Superior Técnico, Universidade de Lisboa, Av. Rovisco Pais, 1049-001, Lisboa, Portugal.
authors.forename: José
authors.initials: J
authors.lastname: Restolho
authors.affiliation: Serviço de Química e Toxicologia Forenses, Instituto Nacional de Medicina Legal e Ciências Forenses, IP - Delegação do Sul, Rua Manuel Bento de Sousa, 3, 1169-201, Lisboa, Portugal.
authors.forename: Mário
authors.initials: M
authors.lastname: Barroso
authors.affiliation: Centro de Química Estrutural do Instituto Superior Técnico, Universidade de Lisboa, Av. Rovisco Pais, 1049-001, Lisboa, Portugal.
authors.forename: Benilde
authors.initials: B
authors.lastname: Saramago
authors.affiliation: Serviço de Química e Toxicologia Forenses, Instituto Nacional de Medicina Legal e Ciências Forenses, IP - Delegação do Sul, Rua Manuel Bento de Sousa, 3, 1169-201, Lisboa, Portugal.
authors.forename: Mário
authors.initials: M
authors.lastname: Dias
authors.affiliation: Research Institute for Medicines and Pharmaceutical Sciences (iMed.ULisboa), Faculdade de Farmácia da Universidade de Lisboa, Av. Prof. Gama Pinto, 1649-003, Lisboa, Portugal.
authors.forename: Carlos A M
authors.initials: CA
authors.lastname: Afonso
mesh_terms: D000701:Analgesics, Opioid / Q000302:isolation & purification*; D006197:Hair / Q000737:chemistry*; D006801:Humans; D052578:Ionic Liquids / Q000737:chemistry*; D009022:Morphine Derivatives / Q000302:isolation & purification*
chemical_list: D000701:Analgesics, Opioid; D052578:Ionic Liquids; D009022:Morphine Derivatives; C026979:6-O-monoacetylmorphine
keywords: DOE; contactless extraction; decontamination; hair; ionic liquids; opiates