title: In-line solid-phase extraction-capillary electrophoresis coupled with mass spectrometry for determination of drugs of abuse in human urine.
abstract: In-line solid-phase extraction-capillary electrophoresis coupled with mass spectrometric detection (SPE-CE-MS) has been used for determination of 2-ethylidene-1,5-dimethyl-3,3-diphenylpyrrolidine (EDDP), codeine (COD), hydrocodeine (HCOD), and 6-acetylmorphine (6AM) in urine. The preconcentration system consists of a small capillary filled with Oasis HLB sorbent and inserted into the inlet section of the electrophoresis capillary. The SPE-CE-MS experimental conditions were optimized as follows: the sample (adjusted to pH 6.0) was loaded at 930 mbar for 60 min, elution was performed with methanol at 50 mbar for 35 s, 60 mmol L(-1) ammonium acetate at pH 3.8 was used as running buffer, the separation voltage was 30 kV, and the sheath liquid at a flow rate of 5.0 μL min(-1) was isopropanol-water 50:50 (v/v) containing 0.5% acetic acid. Analysis of urine samples spiked with the four drugs and diluted 1:1 (v/v) was studied in the linear range 0.08-10 ng mL(-1). Detection limits (LODs) (S/N = 3) were between 0.013 and 0.210 ng mL(-1). Repeatability (expressed as relative standard deviation) was below 7.2%. The method developed enables simple and effective determination of these drugs of abuse in urine samples at the levels encountered in toxicology and doping.
authors.affiliation: Department of Analytical Chemistry and Organic Chemistry, Faculty of Chemistry, Rovira i Virgili University, Marcel·lí Domingo s/n, 43007, Tarragona, Spain.
authors.forename: Igor
authors.initials: I
authors.lastname: Botello
authors.forename: Francesc
authors.initials: F
authors.lastname: Borrull
authors.forename: Marta
authors.initials: M
authors.lastname: Calull
authors.forename: Carme
authors.initials: C
authors.lastname: Aguilar
authors.forename: Govert W
authors.initials: GW
authors.lastname: Somsen
authors.forename: Gerhardus J
authors.initials: GJ
authors.lastname: de Jong
mesh_terms: D003061:Codeine / Q000031:analogs & derivatives / Q000302:isolation & purification / Q000652:urine*; D019075:Electrophoresis, Capillary / Q000379:methods*; D006801:Humans; D013287:Illicit Drugs / Q000302:isolation & purification / Q000652:urine*; D057230:Limit of Detection; D009022:Morphine Derivatives / Q000302:isolation & purification / Q000652:urine*; D011759:Pyrrolidines / Q000302:isolation & purification / Q000652:urine*; D052616:Solid Phase Extraction / Q000379:methods*; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods
chemical_list: D013287:Illicit Drugs; D009022:Morphine Derivatives; D011759:Pyrrolidines; C026979:6-O-monoacetylmorphine; D003061:Codeine; C010724:2-ethylidene-1,5-dimethyl-3,3-diphenylpyrrolidine