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Simoes S.S.,National Institute of Legal Medicine South Branch | Ajenjo A.C.,National Institute of Legal Medicine South Branch | Dias M.J.,National Institute of Legal Medicine South Branch
Rapid Communications in Mass Spectrometry | Year: 2011

A qualitative and quantitative analytical method was developed for the simultaneous determination of δ9-tetrahydrocannabinol (THC), 11-hydroxy-A9-tetrahydrocannabinol (11-OH-THC) and l1-nor-9-carboxy- δ9-tetrahydrocannabinol (THC-COOH) in whole blood. The samples were prepared by solid-phase extraction followed by ultra-performance liquid chromatography/tandem mass spectrometry (UPLC/MS/MS) analysis using positive ion electrospray ionization and multiple reaction monitoring. The chromatographic separation was performed with an Acquity UPLC® HSS T3 (50 × 2.1 mm i.d., 1.8 μm) reversed-phase column using a methanol/2 mM ammonium formate (formic acid 0.1%) gradient in a total run time of 9.5 min. MS/MS detection was achieved with two precursor-product ion transitions per substance. The method was fully validated, including selectivity and capacity of identification, according to the identification criteria (two transitions per substance, signal-tonoise ratio, relative retention time and ion ratio) without the presence of interferences, limit of detection (0.2 μg/L for THC and 0.5 μg/L for 11-OH-THC and THC-COOH), limit of quantitation (0.5 μg/L for all cannabinoids), recovery (53-115%), carryover, matrix effect (34-43%), linearity (0.5-100 μg/L), intra-assay precision (CV < 10% for the relative peak area ratios and <0.1% for the relative retention time), inter-assay accuracy (mean relative error <10%) and precision (CV <11%). The method has already been successfully used in proficiency tests and subsequently applied to authentic samples in routine forensic analysis. Copyright © 2011 John Wiley & Sons, Ltd. Source


Simoes S.S.,National Institute of Legal Medicine South Branch | Ajenjo A.C.,National Institute of Legal Medicine South Branch | Dias M.J.,National Institute of Legal Medicine South Branch
Journal of Pharmaceutical and Biomedical Analysis | Year: 2012

Misoprostol is a pharmaceutical synthetic compound, analog of prostaglandin E1, frequently used as an abortifacient in not medically supervised or self-induced abortions, particularly in countries with restrictive abortion laws representing a serious public health problem. The aim of this study was to develop and validate a sensitive analytical method for the determination of misoprostol acid in whole blood samples. The samples were prepared by SPE and the chromatographic separation was performed by UPLC-MS/MS using ESI- and MRM mode with an Acquity UPLC® BEH C18 (50mm×2.1mm i.d., 1.7μm) column using a methanol-ammonium 0.1% solution gradient in a total run time of 7.0min. The method showed to be selective and linear in range 25-2000ng/L. The LOD and LOQ were 10ng/L and 25ng/L, respectively. The recovery ranged from 89 to 97%. No carryover and significant matrix effect were observed. The intra- and inter-assay precisions and the inter-assay accuracy results were 4.0% and 5.4%, 5.5% and 4.1%, and -1.4% and -2.8%, for the concentrations 50 and 500ng/L, respectively. The method developed allows the analysis of misoprostol acid in whole blood samples with adequate sensitivity to the concentration range obtained from therapeutic doses. The method was successfully used in a controlled misoprostol administration study and has been applied in our laboratory in the forensic toxicology field. © 2012 Elsevier B.V. Source

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