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Ternary mixed-mode silica sorbent of solid-phase extraction for determination of basic, neutral and acidic drugs in human serum

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Abstract

In this study, a ternary mixed-mode silica sorbent (TMSS) with octamethylene, carboxyl, and amino groups was prepared via Cu(I)-catalyzed azide-alkyne cycloaddition (CuAAC) click reaction and a subsequent reduction of azide to primary amine. While used in solid-phase extraction (SPE), the retention behavior of TMSS towards a total of nine kinds of basic, neutral, and acidic drugs was investigated in detail. The results revealed that hydrophobic, ion-exchange interaction, and electrostatic repulsion between TMSS and the analytes were closely related to the retention behavior of TMSS. Besides, the log Kow value of the analyte was also a factor influencing the retention behavior of analytes on TMSS. The nine analytes could be retained by TMSS simultaneously and then, were eluted into two fractions according to the acid-base property of the analytes for further determinations. The acidic and neutral analytes were in one fraction, and the basic ones in the other fraction. When used to treat the human serum spiked with the nine drugs, TMSS offered higher recoveries than BakerBond CBA and comparable recoveries to Oasis WCX. It should be noted TMSS had better purifying capability for human serum than Oasis WCX. Under the optimized SPE conditions, a method of SPE hyphenated to high-performance liquid chromatography-ultraviolet detection (HPLC-UV) for determination of the basic, neutral, and acidic drugs spiked in human serum was established. For the nine drugs, the linear ranges were all between 5.0 and 1000 μg L−1 with correlation coefficients (R2) above 0.9990, and the limits of detection (LODs) were in the range of 0.8–2.3 μg L−1. The intra-day and inter-day relative standard deviations (RSDs) were less than 5.3 and 8.8%, respectively.

Treating drugs in human serum by SPE with ternary mixed-mode silica sorbent.

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Authors and Affiliations

  1. Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan, 430072, Hubei, China

    Shupei Jin & Jun Xing

  2. Kaifeng Inspection Center for Agricultural Products Safety and Quality, Kaifeng, 475000, Henan, China

    Shupei Jin

  3. Guangdong Communication Polytechnic Education Center, Guangzhou, 510650, Guangdong, China

    Yinghua Qiao

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  1. Shupei Jin
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  2. Yinghua Qiao
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  3. Jun Xing
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Correspondence to Jun Xing.

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The study has been approved by the Hospital of Wuhan University Ethics Committee and has been performed in accordance with the ethical standards.

Informed consent was obtained from all individual participants included in the study.

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The authors declare that there is no conflict of interest and all the authors have materially participated in the research and/or article preparation.

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Jin, S., Qiao, Y. & Xing, J. Ternary mixed-mode silica sorbent of solid-phase extraction for determination of basic, neutral and acidic drugs in human serum. Anal Bioanal Chem 410, 3731–3742 (2018). https://doi.org/10.1007/s00216-018-1037-3

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  • DOI: https://doi.org/10.1007/s00216-018-1037-3

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