title: Direct injection determination of benzoylecgonine, heroin, 6-monoacetylmorphine and morphine in serum by MLC.
abstract: A simple and sensitive direct injection chromatographic procedure is developed for the determination of heroin, two of its metabolites (morphine and 6-monoacetylmorphine (6-MAM)), and benzoylecgonine (a metabolite of cocaine) in serum samples. The proper resolution of the four substances is obtained with a chemometrics approach, where the retention is modelled as a first step using the retention factors obtained in a limited number of mobile phases. Afterwards, an optimisation criterion that takes into account the position and shape of the chromatographic peaks is applied. The mobile phase selected to carry out the analysis was 0.1 mol L(-1) SDS-4% (v/v) butanol buffered at pH 7, in which the separation is performed in less than 18 min. The limits of quantification were in the 17-36 ng mL(-1) range. Intra- and inter-day assay accuracy and precision (below 3%) were obtained following ICH guidelines. The method developed was applied to the determination of the drugs studied in serum samples with good recoveries (90-104%). Serum samples from subjects that have been ingested cocaine and heroin were also analysed. The samples were injected directly in the chromatographic system without any pretreatment.
authors.affiliation: Area de Química Analítica, Universitat Jaume I, Campus Riu Sec, 12080 Castelló, Spain.
authors.forename: Maria-Elisa
authors.initials: ME
authors.lastname: Capella-Peiró
authors.forename: Devasish
authors.initials: D
authors.lastname: Bose
authors.forename: Mayte
authors.initials: M
authors.lastname: Gil-Agustí
authors.forename: Josep
authors.initials: J
authors.lastname: Esteve-Romero
authors.forename: Samuel
authors.initials: S
authors.lastname: Carda-Broch
mesh_terms: D002853:Chromatography, Liquid / Q000379:methods*; D003042:Cocaine / Q000031:analogs & derivatives* / Q000097:blood*; D003932:Heroin / Q000097:blood*; D008823:Micelles; D009020:Morphine / Q000097:blood*; D009022:Morphine Derivatives / Q000097:blood*; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity
chemical_list: D008823:Micelles; D009022:Morphine Derivatives; C005618:benzoylecgonine; D003932:Heroin; D009020:Morphine; D003042:Cocaine; C026979:6-O-monoacetylmorphine