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
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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.
KeywordsOn-line SPE-HPLC Polymer monolithic sorbent Dioscin Dioscorea nipponica rhizome Ethylene glycol phenyl ether acrylate
Ethylene glycol dimethacrylate
High-performance liquid chromatography
Ethylene glycol phenyl ether acrylate
Scanning electron microscopy
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.
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 was obtained for experimentation and submission from the volunteer and each of the co-authors.
- 5.Shen CY, Jiang JG, Yang L, Wang DW, Zhu W. Anti-ageing active ingredients from herbs and nutraceuticals used in traditional Chinese medicine: pharmacological mechanisms and implications for drug discovery. Brit J Pharmacol. 2017;174(11):1395–425. https://doi.org/10.1111/bph.13631.CrossRefGoogle Scholar
- 13.Liu J, Yang X, Li L, Zhang Q, Zhang Z, Zhang X, et al. A rapid and sensitive liquid chromatography–tandem mass spectrometric method for the determination of hederasaponin B in rat plasma: application to a pharmacokinetic study. Asian J Pharm Sci. 2017;12(4):363–9. https://doi.org/10.1016/j.ajps.2016.09.001.CrossRefGoogle Scholar
- 15.Marchioni C, de Souza ID, Acquaro VR, de Souza Crippa JA, Tumas V, Queiroz MEC. Recent advances in LC-MS/MS methods to determine endocannabinoids in biological samples: application in neurodegenerative diseases. Anal Chim Acta. 2018;1044:12–28. https://doi.org/10.1016/j.aca.2018.06.016.CrossRefPubMedGoogle Scholar
- 20.Lin SL, Wu YR, Lin TY, Fuh MR. Preparation and evaluation of poly(alkyl methacrylate-co-methacrylic acid-co-ethylene dimethacrylate) monolithic columns for separating polar small molecules by capillary liquid chromatography. Anal Chim Acta. 2015;871:57–65. https://doi.org/10.1016/j.aca.2015.02.015.CrossRefPubMedGoogle Scholar
- 21.Li X, Wang MM, Zheng GY, Ai LF, Wang XS. Fast and online determination of five avermectin residues in foodstuffs of plant and animal origin using reusable polymeric monolithic extractor coupled with LC-MS/MS. J Agric Food Chem. 2015;63(16):4096–103. https://doi.org/10.1021/acs.jafc.5b00739.CrossRefPubMedGoogle Scholar
- 23.Lan D, Bai L, Pang X, Liu H, Yan H, Guo H. In situ synthesis of a monolithic material with multi-sized pores and its chromatographic properties for the separation of intact proteins from human plasma. Talanta. 2019;194:406–14. https://doi.org/10.1016/j.talanta.2018.10.054.CrossRefPubMedGoogle Scholar
- 24.Yang G, Lu W, Pan M, Zhang C, Zhou Y, Hu P, et al. An LC–MS/MS method for simultaneous determination of nine steroidal saponins from Paris polyphylla var. in rat plasma and its application to pharmacokinetic study. J Pharm Biomed Anal. 2017;145:675–81. https://doi.org/10.1016/j.jpba.2017.07.052.CrossRefGoogle Scholar
- 28.Zhang X, Li J, Ito Y, Sun W. Simultaneous quantification of five steroid saponins from Dioscorea zingiberensis C.H. Wright in rat plasma by HPLC–MS/MS and its application to the pharmacokinetic studies. Steroids. 2015;93:16–24. https://doi.org/10.1016/j.steroids.2014.08.023.CrossRefPubMedGoogle Scholar