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A rapid method for on-line solid-phase extraction and determination of dioscin in human plasma using a homemade monolithic sorbent combined with high-performance liquid chromatography

  • Shan Peng
  • Ligai BaiEmail author
  • Xiaoqian Shi
  • Mingxue Li
  • Laisen Wang
  • Fanrong Sun
  • Haiyan Liu
Research Paper
  • 21 Downloads

Abstract

A phenyl-based polymer monolithic column was prepared via free radical polymerization in a stainless steel column with the size of 4.6 mm i.d. × 50 mm, using ethylene glycol phenyl ether acrylate as the monomer. The resulting monolithic column shows high porosity of 73.42% and relative uniform pore structure, as characterized by mercury porosimetry and scanning electron microscopy, respectively. The optimized polymer monolith column was used for on-line solid-phase extraction prior to the reversed phase mode HPLC-UV analysis for the determination of dioscin in human plasma, using a COSMOSIL C18 column (4.6 mm × 150 mm, 4.5 μm). Water was used to wash non-retained components from the SPE sorbent, and methanol water (80:20, V/V) was used as the mobile phase for isocratic elution of dioscin. The maximum adsorbed quantity of dioscin to the SPE column is 6.79 mg/g, which is high enough for the quantitative analysis of dioscin in plasma, due to the low content of dioscin in plasma. The method was validated by assessing the linearity, lower limit of quantification, intra- and inter-day precision, accuracy, and repeatability. The developed method was applied for the analysis of dioscin in plasma from a volunteer who had orally administered an aqueous extract of dioscorea nipponica rhizome, showing the method capable of detecting dioscin in the plasma. These results show that the developed method is a rapid method for on-line solid-phase extraction and determination of dioscin from plasma, exhibiting good selectivity with hydrogen bond interaction and hydrophobic interaction, good clean-up ability, cost-saving, and time-saving.

Graphical abstract

Keywords

On-line SPE-HPLC Polymer monolithic sorbent Dioscin Dioscorea nipponica rhizome Ethylene glycol phenyl ether acrylate 

Abbreviations

ACN

Acetonitrile

AIBN

Azobisisobutyronitrile

BET

Brunauer-Emmett-Teller

DMF

N,N-Dimethylformamide

EDMA

Ethylene glycol dimethacrylate

HPLC

High-performance liquid chromatography

PHEA

Ethylene glycol phenyl ether acrylate

SEM

Scanning electron microscopy

SPE

Solid-phase extraction

TMPTA

Trimethylolpropane triacrylate

Notes

Funding information

This work was supported by the National Natural Science Foundation of China (Grant Numbers 21505030 and 21575033).

Compliance with Ethical Standards

Conflict of interest

The authors declare that they have no conflicts of interest.

Ethical approval

All experiments were in accordance with the ethical guidelines for biomedical research involving human subjects (for Trial Implementation), Ministry of health, China, and approved by the institutional ethical committee of Hebei University.

Informed consent

Informed consent was obtained for experimentation and submission from the volunteer and each of the co-authors.

Supplementary material

216_2019_2256_MOESM1_ESM.pdf (1.1 mb)
ESM 1 (PDF 1075 kb)

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Copyright information

© Springer-Verlag GmbH Germany, part of Springer Nature 2019

Authors and Affiliations

  1. 1.College of Pharmaceutical SciencesHebei UniversityBaodingChina
  2. 2.Key Laboratory of Medicinal Chemistry and Molecular Diagnosis, Ministry of EducationHebei UniversityBaodingChina

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