title: Optimization of a rapid microwave-assisted extraction method for the simultaneous determination of opiates, cocaine and their metabolites in human hair.
abstract: A rapid and cleanup-free microwave-assisted extraction (MAE) method is proposed for the simultaneous extraction of six illegal drugs of abuse - cocaine, benzoylecgonine (BZE), cocaethylene (CCE), morphine, 6-monoacethylmorphine (6AM) and codeine - from human hair samples. The analytes were determined using high performance liquid chromatography (HPLC) with photodiode array UV detection. The influence of several variables on the efficiency of the MAE procedure was investigated in detail by a multi-objective optimization approach based on a hybrid experimental design (17 experiments) and desirability functions. Six drugs were successfully extracted from human hair with recoveries close to 100% and good reproducibility (<3.6% RSD) under the optimal MAE conditions: 11 mL dichloromethane (DCM) extraction solvent, 60 degrees C extraction temperature, 9 min extraction time and 0.5 mL of methanol (MeOH) added to 50mg of the hair sample in the extraction vessels. Limits of quantification of 0.2 ng mg(-1) were found for the studied compounds. A comparison of sample preparation procedures, including MAE, enzymatic digestion and digestion by aqueous acids, was also conducted. The results indicated that the global behaviour of sample procedures provided similar satisfactory recoveries ranging from 86 to 100%. Indeed, the MAE procedure resulted in a reduction of extraction time by 100-fold and the elimination of cleanup steps. Slightly higher recoveries of morphine, 6AM, BZE and CCE, at 1 ng mg(-1) concentration level and cocaine at 40 ng mg(-1) concentration level, were achieved using MAE. Lastly, the proposed MAE method was applied to several human hair samples from multidrug abusers.
authors.affiliation: Institute of Legal Medicine, Forensic Toxicology Service, Faculty of Medicine, University of Santiago de Compostela, Spain.
authors.forename: P
authors.initials: P
authors.lastname: Fernández
authors.forename: M
authors.initials: M
authors.lastname: Lago
authors.forename: R A
authors.initials: RA
authors.lastname: Lorenzo
authors.forename: A M
authors.initials: AM
authors.lastname: Carro
authors.forename: A M
authors.initials: AM
authors.lastname: Bermejo
authors.forename: M J
authors.initials: MJ
authors.lastname: Tabernero
mesh_terms: D000701:Analgesics, Opioid / Q000032:analysis*; D002851:Chromatography, High Pressure Liquid / Q000379:methods; D003042:Cocaine / Q000031:analogs & derivatives / Q000032:analysis; D003061:Codeine / Q000032:analysis; D006197:Hair / Q000737:chemistry*; D006801:Humans; D013287:Illicit Drugs / Q000032:analysis*; D008872:Microwaves; D009020:Morphine / Q000032:analysis; D009022:Morphine Derivatives / Q000032:analysis; D009294:Narcotics / Q000032:analysis*
chemical_list: D000701:Analgesics, Opioid; D013287:Illicit Drugs; D009022:Morphine Derivatives; D009294:Narcotics; C005618:benzoylecgonine; D009020:Morphine; C066444:cocaethylene; D003042:Cocaine; C026979:6-O-monoacetylmorphine; D003061:Codeine