Regional Centre of Advanced Technologies and Materials, Department of Analytical Chemistry, Faculty of Science, Palacký University in Olomouc, 17. Listopadu 12, Olomouc CZ-77146, Czech Republic.
Department of Forensic Medicine and Medical Law, Faculty Hospital, Hněvotínská 3, Olomouc CZ-77515, Czech Republic.
J Chromatogr A. 2014 Aug 22;1356:258-65. doi: 10.1016/j.chroma.2014.06.058. Epub 2014 Jun 25.
A micellar electrokinetic chromatography method with tandem mass spectrometry has been developed for the selective separation, identification and determination of twelve new designer drugs from the group of synthetic cathinones. Ammonium salt of perfluorooctanoic acid at various concentrations as a volatile background electrolyte (BGE) to create micellar phase was studied for separation of selected synthetic cathinones with direct tandem mass spectrometry without significant loss of detection sensitivity. The optimized BGE contained 100 mM perfluorooctanoic acid with 200 mM ammonium hydroxide providing acceptable resolution of studied drugs in the MEKC step. In order to minimize interferences with matrix components and to preconcentrate target analytes, solid phase extraction was introduced as a clean-up step. The method was linear in the concentration range of 10-5000 ng mL(-1) and the limits of detection were in the range of 10-78 ng mL(-1). The method was demonstrated to be specific, sensitive, and reliable for the systematic toxicological analysis of these derivatives in urine samples.
建立了一种胶束电动色谱-串联质谱法,用于选择性分离、鉴定和测定合成卡西酮类中的 12 种新型设计药物。研究了不同浓度的全氟辛酸铵盐作为挥发性背景电解质(BGE),以创建胶束相,用于直接串联质谱法分离选定的合成卡西酮,而不会显著降低检测灵敏度。优化的 BGE 包含 100mM 全氟辛酸和 200mM 氨,可在 MEKC 步骤中提供研究药物的可接受分辨率。为了最大程度减少基质成分的干扰并预浓缩目标分析物,引入固相萃取作为净化步骤。该方法在 10-5000ng/mL 的浓度范围内呈线性,检测限范围为 10-78ng/mL。该方法在尿液样品中对这些衍生物的系统毒理学分析中表现出特异性、灵敏性和可靠性。