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An etched polyether ether ketone tube covered with immobilized graphene oxide for online solid phase microextraction of quaternary alkaloids prior to their quantitation by HPLC-MS/MS

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Abstract

Polyether ether ketone (PEEK) is an ideal substrate for in tube solid-phase microextraction (SPME) because it overcomes the shortcomings of conventional silica fibers in terms of fragility and poor flexibility. Commonly used bare PEEK tubes suffer from difficult modification with selective sorbents and low inner surface areas. This problem was solved by etching with concentrated sulfuric acid, which dissolves the amorphous regions of the PEEK surface and yields a rough inner surface with plenty of microscopically small holes. The etched tube was then stepwise functionalized with polydopamine and graphene oxide which was in-situ immobilized. The modified tube displays excellent efficiency for the extraction of positively charged quaternary alkaloids by a mixed-mode extraction. Enrichment factors from 221 to 275 can be obtained for the extraction of the alkaloids jatrorrhizine, palmatine and berberine. The alkaloiods were then quantified by online SPME-HPLC-MS/MS detection. The method has detection limits of 0.1 pg mL−1, good linearity, and good intra-day reproducibility (≤ 2.4%). It was applied to the analysis of the three alkaloids in Cortex Phellodendri herb and rat plasma after oral administration.

A concentrated sulfuric acid etching method was used for enhance the workability of polyether ether ketone tube (PEEK) in solid phase microextraction (SPME). The etched tube was covered with graphene oxide (GO) for extraction of protoberberines.

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Acknowledgements

This work was supported by the National Natural Science Foundation of China (Grant nos. 21375101, 81573384 and 91417301) and Natural Science Foundation of Hubei Province (No. 2014CFA077).

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Author notes

  1. Chenlu Wang and Wei Zhou have contributed equally to this work.

Authors and Affiliations

  1. Key Laboratory of Combinatorial Biosynthesis and Drug Discovery, Ministry of Education, and Wuhan University School of Pharmaceutical Sciences, Wuhan, 430071, China

    Chenlu Wang, Wei Zhou, Xiaoyan Liao & Zilin Chen

  2. State Key Laboratory of Transducer Technology, Chinese Academy of Sciences, Beijing, 10080, China

    Chenlu Wang, Wei Zhou & Zilin Chen

  3. Weldon School of Biomedical Engineering, Purdue University, West Lafayette, IN, 47907, USA

    Wenpeng Zhang

Authors
  1. Chenlu Wang
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  2. Wei Zhou
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  3. Xiaoyan Liao
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  4. Wenpeng Zhang
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  5. Zilin Chen
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Correspondence to Zilin Chen.

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Wang, C., Zhou, W., Liao, X. et al. An etched polyether ether ketone tube covered with immobilized graphene oxide for online solid phase microextraction of quaternary alkaloids prior to their quantitation by HPLC-MS/MS. Microchim Acta 184, 2715–2721 (2017). https://doi.org/10.1007/s00604-017-2262-8

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  • DOI: https://doi.org/10.1007/s00604-017-2262-8

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