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Enantiomeric determination of cathinones in environmental water samples by liquid chromatography-high resolution mass spectrometry.
Journal of Chromatography A ( IF 3.8 ) Pub Date : 2020-06-20 , DOI: 10.1016/j.chroma.2020.461359
Yandi Fu 1 , Francesc Borrull 1 , Rosa Maria Marcé 1 , Núria Fontanals 1
Affiliation  

The enantiomeric determination of chiral drugs in the environment is of emerging concern since their enantiomers often exhibit stereoselectivity in environmental occurrence, fate and toxicity. In this study a method based on solid-phase extraction followed by chiral liquid chromatography and high-resolution mass spectrometry has been developed for the enantiomeric determination of a group of cathinones in river water and effluent wastewater. The enantioseparation was carried out using a Chiralpak CBH column in reversed-phase mode, and optimised by evaluating the effects of flow rate, buffer concentration and organic modifier. Under optimal conditions, good enantioseparations (Rs ≥1.2) were achieved for all the analytes. Two mixed-mode cation-exchange sorbents (Oasis WCX and Oasis MCX) in solid-phase extraction were evaluated in river water. Oasis MCX sorbent showed better performance with apparent recoveries ranging from 57 to 91% and matrix effect ranging from -10 to 15%. It is worth noting that a shifting of retention times and loss of enantioresolutions in environmental water samples was observed for all the analytes when the Oasis WCX sorbent was used. The method was validated with river water and effluent wastewater samples and its overall performance was satisfactory. The method quantification limits for all the analyte enantiomers ranged from 1.0 to 2.9 ng/L in river water, and from 2.3 to 6.0 ng/L in effluent wastewater. The repeatability and reproducibility values, expressed as% relative standard deviation (n = 5) were less than 15%. The method was then applied to the analysis of river water and effluent wastewater. The racemic methylone and methedrone (EF=0.49 and 0.46, respectively) were detected at low ng/L in some of the river water samples.



中文翻译:

液相色谱-高分辨率质谱法测定环境水样中的卡西酮对映体。

环境中手性药物的对映异构体测定正引起人们的关注,因为它们的对映异构体在环境发生,命运和毒性方面通常表现出立体选择性。在这项研究中,已开发出一种基于固相萃取,手性液相色谱和高分辨率质谱的方法,用于对映体测定河水和废水中的一系列卡西酮。对映体分离使用Chiralpak CBH色谱柱以反相模式进行,并通过评估流速,缓冲液浓度和有机改性剂的影响进行优化。在最佳条件下,良好的对映体分离(R s所有分析物均达到≥1.2)。在河水中评估了固相萃取中的两种混合模式阳离子交换吸附剂(Oasis WCX和Oasis MCX)。Oasis MCX吸附剂表现出更好的性能,表观回收率介于57%至91%之间,基质效应介于-10%至15%之间。值得注意的是,使用Oasis WCX吸附剂时,对于所有分析物,在环境水样品中均会观察到保留时间的变化和对映体分辨率的损失。对该方法进行了河流水和废水废水样品的验证,其整体性能令人满意。所有分析物对映体的方法定量限在河水中为1.0到2.9 ng / L,在废水中为2.3到6.0 ng / L。重复性和再现性值,表示为相对标准偏差的百分比(n  = 5)小于15%。然后将该方法应用于河流水和废水的分析。在某些河流水样中,以低ng / L的浓度检测到外消旋甲酮和甲氧麻黄酮(分别为EF = 0.49和0.46)。

更新日期:2020-06-27
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