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基于超高效超临界流体色谱串联质谱法对环境样品中选定药物进行对映体选择性同步分析。

Enantioselective simultaneous analysis of selected pharmaceuticals in environmental samples by ultrahigh performance supercritical fluid based chromatography tandem mass spectrometry.

作者信息

Camacho-Muñoz Dolores, Kasprzyk-Hordern Barbara, Thomas Kevin V

机构信息

Department of Chemistry, University of Bath, Bath, BA2 7AY, United Kingdom.

Department of Chemistry, University of Bath, Bath, BA2 7AY, United Kingdom.

出版信息

Anal Chim Acta. 2016 Aug 31;934:239-51. doi: 10.1016/j.aca.2016.05.051. Epub 2016 Jun 4.

Abstract

In order to assess the true impact of each single enantiomer of pharmacologically active compounds (PACs) in the environment, highly efficient, fast and sensitive analytical methods are needed. For the first time this paper focuses on the use of ultrahigh performance supercritical fluid based chromatography coupled to a triple quadrupole mass spectrometer to develop multi-residue enantioselective methods for chiral PACs in environmental matrices. This technique exploits the advantages of supercritical fluid chromatography, ultrahigh performance liquid chromatography and mass spectrometry. Two coated modified 2.5 μm-polysaccharide-based chiral stationary phases were investigated: an amylose tris-3,5-dimethylphenylcarbamate column and a cellulose tris-3-chloro-4-methylphenylcarbamate column. The effect of different chromatographic variables on chiral recognition is highlighted. This novel approach resulted in the baseline resolution of 13 enantiomers PACs (aminorex, carprofen, chloramphenicol, 3-N-dechloroethylifosfamide, flurbiprofen, 2-hydroxyibuprofen, ifosfamide, imazalil, naproxen, ofloxacin, omeprazole, praziquantel and tetramisole) and partial resolution of 2 enantiomers PACs (ibuprofen and indoprofen) under fast-gradient conditions (<10 min analysis time). The overall performance of the methods was satisfactory. The applicability of the methods was tested on influent and effluent wastewater samples. To the best of our knowledge, this is the first feasibility study on the simultaneous separation of chemically diverse chiral PACs in environmental matrices using ultrahigh performance supercritical fluid based chromatography coupled with tandem mass spectrometry.

摘要

为了评估环境中具有药理活性化合物(PACs)的每种对映体的真实影响,需要高效、快速且灵敏的分析方法。本文首次聚焦于使用基于超高效超临界流体的色谱与三重四极杆质谱联用,来开发用于环境基质中手性PACs的多残留对映体选择性方法。该技术利用了超临界流体色谱、超高效液相色谱和质谱的优势。研究了两种涂覆改性的2.5μm多糖基手性固定相:直链淀粉三(3,5-二甲基苯基)氨基甲酸酯柱和纤维素三(3-氯-4-甲基苯基)氨基甲酸酯柱。突出了不同色谱变量对手性识别的影响。这种新方法在快速梯度条件下(分析时间<10分钟)实现了13种PACs对映体(阿米雷司、卡洛芬、氯霉素、3-N-脱氯乙基亚磷酰胺、氟比洛芬、2-羟基布洛芬、异环磷酰胺、抑霉唑、萘普生、氧氟沙星、奥美拉唑、吡喹酮和四咪唑)的基线分离以及2种PACs对映体(布洛芬和吲哚洛芬)的部分分离。这些方法的整体性能令人满意。在进水和出水废水样品上测试了这些方法的适用性。据我们所知,这是首次使用基于超高效超临界流体的色谱与串联质谱联用对环境基质中化学性质不同的手性PACs进行同时分离的可行性研究。

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