Skip to main content
SpringerLink
Log in

Development of an SPE Method Using Ionic Liquid-Based Monolithic Column for On-Line Cleanup of Human Plasma and Simultaneous Determination of Five Steroid Drugs

  • Original
  • Published:
Chromatographia Aims and scope Submit manuscript

Abstract

An 1-vinyl-3-hexyl imidazolium bromide ionic liquid-based monolithic column was prepared via in situ free radical polymerization, which was used as the sorbent of on-line solid phase extraction. The prepared material was characterized by scanning electron microscopy, nitrogen adsorption–desorption instrument and mercury intrusion porosimetry, respectively, and the results showed that the homemade monolith occupied relatively uniform porous structure and high-specific surface area of 212.53 m2 g−1. On-line solid phase extraction–high-performance liquid chromatography was performed to quantitatively analyze five steroid drugs, including betamethasone, norgestrel, halcinonide, beclomethasone dipropionate and testosterone propionate in human plasma. The determination procedure was carried out following the optimization of the mobile phase composition. Methodological validation showed that correlation coefficients of the linear regressions were in the range of 0.9989–0.9992; the values of relative standard deviation for precision were in the range of 1.39–6.15% for intra-day and 0.32–6.34% for inter-day, respectively; the values of accuracy expressed by recovery were in the range of 99.02–101.98, 93.27–102.89, 102.79–104.01, 100.04–102.61 and 100.77–102.44% for the five drugs in order, respectively; the values of relative standard deviation for repeatability calculated according to retention times and peak areas of the five drugs were in the ranges of 0.28–0.76% (n = 5) and 0.84–2.63% (n = 5), respectively. The results showed that the polymer monolithic column was feasible for an on-line solid phase extraction column, exhibiting good selectivity and high permeability.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Log in via an institution

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Institutional subscriptions

Fig. 1
Fig. 2
Fig. 3
Fig. 4
Fig. 5

Similar content being viewed by others

References

  1. El-Desoky E-SI, Reyad M, Afsah EM, Dawidar A-AM (2016) Synthesis and chemical reactions of the steroidal hormone 17 α-methyltestosterone. Steroids 105:68–95

    Article  CAS  Google Scholar 

  2. Nguyen ET, Caldwell JL, Streicher J, Ghisays V, Balmer NJ, Estrada CM, Solomon MB (2018) Differential effects of imipramine and CORT118335 (Glucocorticoid receptor modulator/mineralocorticoid receptor antagonist) on brain-endocrine stress responses and depression-like behavior in female rats. Behav Brain Res 336:99–110

    Article  CAS  PubMed  Google Scholar 

  3. Schulz KM, Sisk CL (2016) The organizing actions of adolescent gonadal steroid hormones on brain and behavioral development. Neurosci Biobehav Rev 70:148–158

    Article  CAS  PubMed  PubMed Central  Google Scholar 

  4. Caplan A, Fett N, Rosenbach M, Werth VP, Micheletti RG (2017) Prevention and management of glucocorticoid-induced side effects: a comprehensive review: ocular, cardiovascular, muscular, and psychiatric side effects and issues unique to pediatric patients. J Am Acad Dermatol 76:201–207

    Article  PubMed  Google Scholar 

  5. Konieczna L, Belka M, Okońska M, Pyszka M, Bączek T (2018) New 3D-printed sorbent for extraction of steroids from human plasma preceding LC–MS analysis. J Chromatogr A 1545:1–11

    Article  CAS  PubMed  Google Scholar 

  6. Szeitz A, Manji J, Riggs KW, Thamboo A, Javer AR (2014) Validated assay for the simultaneous determination of cortisol and budesonide in human plasma using ultra high performance liquid chromatography–tandem mass spectrometry. J Pharm Biomed 90:198–206

    Article  CAS  Google Scholar 

  7. Matysik S, Liebisch G (2017) Quantification of steroid hormones in human serum by liquid chromatography-high resolution tandem mass spectrometry. J Chromatogr A 1526:112–118

    Article  CAS  PubMed  Google Scholar 

  8. Appelblad P, Irgum K (2002) Separation and detection of neuroactive steroids from biological matrices. J Chromatogr A 955:151–182

    Article  CAS  PubMed  Google Scholar 

  9. Sakamoto Y, Jinno Y, Shinodzuka I, Iwasaki Y, Ito R, Saito K (2014) Sample cleanup using solid-phase dispersive extraction for determination of vancomycin in serum. Anal Sci 30:271–275

    Article  CAS  PubMed  Google Scholar 

  10. Lamei N, Ezoddin M, Abdi K (2017) Air assisted emulsification liquid-liquid microextraction based on deep eutectic solvent for preconcentration of methadone in water and biological samples. Talanta 165:176–181

    Article  CAS  PubMed  Google Scholar 

  11. Wang NN, Xin HL, Zhang QY, Jiang YP, Wang XP, Shou D, Qin LP (2017) Carbon nanotube-polymer composite for effervescent pipette tip solid phase microextraction of alkaloids and flavonoids from Epimedii herba in biological samples. Talanta 162:10–18

    Article  CAS  PubMed  Google Scholar 

  12. Martins PF, de Melo MMR, Sarmento P, Silva CM (2016) Supercritical fluid extraction of sterols from Eichhornia crassipes biomass using pure and modified carbon dioxide. Enhancement of stigmasterol yield and extract concentration. J Supercrit Fluid 107:441–449

    Article  CAS  Google Scholar 

  13. Wu FL, Xu CS, Jiang N, Wang JB, Ding CF (2018) Poly (methacrylic acid-co-diethenyl-benzene) monolithic microextraction column and its application to simultaneous enrichment and analysis of mycotoxins. Talanta 178:1–8

    Article  CAS  PubMed  Google Scholar 

  14. Saito K, Kikuchi Y, Saito R (2014) Solid-phase dispersive extraction method for analysis of benzodiazepine drugs in serum and urine samples. J Pharm Biomed 100:28–32

    Article  CAS  Google Scholar 

  15. Yang MY, Gu YH, Wu XL, Xi XF, Yang XL, Zhou WF, Zeng HZ, Zhang SB, Lu RH, Gao HX, Li J (2018) Rapid analysis of fungicides in tea infusions using ionic liquid immobilized fabric phase sorptive extraction with the assistance of surfactant fungicides analysis using IL-FPSE assisted with surfactant. Food Chem 239:797–809

    Article  CAS  PubMed  Google Scholar 

  16. Łuczak J, Paszkiewicz M, Krukowska A, Malankowska A, Zaleska-Medynska A (2016) Ionic liquids for nano- and microstructures preparation. Part 1: properties and multifunctional role. Adv Colloid Interfac 230:13–28

    Article  CAS  Google Scholar 

  17. Tang S, Liu SJ, Guo Y, Liu X, Jiang SX (2014) Recent advances of ionic liquids and polymeric ionic liquids in capillary electrophoresis and capillary electrochromatography. J Chromatogr A 1357:147–157

    Article  CAS  PubMed  Google Scholar 

  18. Han HF, Wang Q, Liu X, Jiang SX (2012) Polymeric ionic liquid modified organic-silica hybrid monolithic column for capillary electrochromatography. J Chromatogr A 1246:9–14

    Article  CAS  PubMed  Google Scholar 

  19. Ali I, Suhail M, Sanagi MM, Aboul-Enein HY (2017) Ionic liquids in HPLC and CE: a hope for future. Crit Rev Anal Chem 47:332–339

    Article  CAS  PubMed  Google Scholar 

  20. Liu S, Wang CL, He S, Bai LG, Liu HY (2016) On-line SPE using ionic liquid-based monolithic column for the determination of antihypertensives in human plasma. Chromatographia 79:441–449

    Article  CAS  Google Scholar 

  21. Liu S, Zong JX, Wei Z, Zhang H, Bai LG, Liu HY, Yan HY (2016) Determination of trace macrolide antibiotics in milk with online solid phase extraction with an ionic-liquid-based monolithic column. J Appl Polym Sci 133:43943

    Google Scholar 

  22. Obbed MS, Aqel A, Al Othman ZA, Badjah-Hadj-Ahmed A-Y (2018) Preparation, characterization and application of polymethacrylate-based monolithic columns for fast and efficient separation of alkanes, alcohols, alkylbenzenes and isomeric mixtures by gas chromatography. J Chromatogr A 1555:89–99

    Article  CAS  PubMed  Google Scholar 

  23. Qin ZN, Yu QW, Wang RQ, Feng YQ (2018) Preparation of polymer monolithic column functionalized by arsonic acid groups for mixed-mode capillary liquid chromatography. J Chromatogr A 1547:21–28

    Article  CAS  PubMed  Google Scholar 

  24. Ma SJ, Zhang HY, Li Y, Li YN, Zhang N, Ou JJ, Ye ML, Wei YM (2018) Fast preparation of hybrid monolithic columns via photo-initiated thiol-yne polymerization for capillary liquid chromatography. J Chromatogr A 1538:8–16

    Article  CAS  PubMed  Google Scholar 

  25. Ponzetto F, Boccard J, Baume N, Kuuranne T, Rudaz S, Saugy M, Nicoli R (2017) High-resolution mass spectrometry as an alternative detection method to tandem mass spectrometry for the analysis of endogenous steroids in serum. J Chromatogr B 1052:34–42

    Article  CAS  Google Scholar 

  26. Caron P, Turcotte V, Guillemette C (2015) A chromatography/tandem mass spectrometry method for the simultaneous profiling of ten endogenous steroids, including progesterone, adrenal precursors, androgens and estrogens, using low serum volume. Steroids 104:16–24

    Article  CAS  PubMed  Google Scholar 

  27. Quanson JL, Stander MA, Pretorius E, Jenkinson C, Taylor AE, Storbeck KH (2016) High-throughput analysis of 19 endogenous androgenic steroids by ultra-performance convergence chromatography tandem mass spectrometry. J Chromatogr B 1031:131–138

    Article  CAS  Google Scholar 

  28. Frey AJ, Wang QQ, Busch C, Feldman D, Bottalico L, Mesaros CA, Blair IA, Vachani A, Snyder NW (2016) Validation of highly sensitive simultaneous targeted and untargeted analysis of keto-steroids by Girard P derivatization and stable isotope dilution-liquid chromatography-high resolution mass spectrometry. Steroids 116:60–66

    Article  CAS  PubMed  PubMed Central  Google Scholar 

  29. Robles J, Marcos J, Renau N, Garrostas L, Segura J, Ventura R, Barceló B, Barceló A, Pozo OJ (2017) Quantifying endogenous androgens, estrogens, pregnenolone and progesterone metabolites in human urine by gas chromatography tandem mass spectrometry. Talanta 169:20–29

    Article  CAS  PubMed  Google Scholar 

  30. Li H, Ai LF, Fan SF, Wang Y, Sun DX (2017) Rapid determination of 18 glucocorticolds in serum using reusable on-line SPE polymeric monolithic column coupled with LC-quadrupole/orbitrap high-resolution mass spectrometer. J Chromatogr B 1065–1066:79–86

    Article  CAS  Google Scholar 

Download references

Acknowledgements

This work was supported by the National Natural Science Foundation of China (Grant numbers 21505030, 21575033) and the Natural Science Foundation of Hebei Province (Grant number H2017201075).

Author information

Authors and Affiliations

  1. College of Pharmaceutical Sciences, Hebei University, Baoding, 071002, Hebei, China

    Xiaomin Pang, Ligai Bai, Dandan Lan, Bin Guo, Huimin Wang, Haiyan Liu & Zhengyue Ma

  2. Key Laboratory of Medicinal Chemistry and Molecular Diagnosis, Ministry of Education, Hebei University, Baoding, 071002, China

    Xiaomin Pang, Ligai Bai, Dandan Lan, Bin Guo, Huimin Wang & Haiyan Liu

  3. Key Laboratory of Pharmaceutical Quality Control of Hebei Province, Hebei University, Baoding, 071002, China

    Xiaomin Pang, Ligai Bai, Dandan Lan, Bin Guo, Huimin Wang, Haiyan Liu & Zhengyue Ma

Authors
  1. Xiaomin Pang
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. Ligai Bai
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. Dandan Lan
    View author publications

    You can also search for this author in PubMed Google Scholar

  4. Bin Guo
    View author publications

    You can also search for this author in PubMed Google Scholar

  5. Huimin Wang
    View author publications

    You can also search for this author in PubMed Google Scholar

  6. Haiyan Liu
    View author publications

    You can also search for this author in PubMed Google Scholar

  7. Zhengyue Ma
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding author

Correspondence to Ligai Bai.

Ethics declarations

Conflict of interest

The authors declared that there is no conflict of interest.

Informed consent

Informed consent was obtained from all the subjects.

Electronic supplementary material

Below is the link to the electronic supplementary material.

Supplementary material 1 (DOCX 13910 KB)

Rights and permissions

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Pang, X., Bai, L., Lan, D. et al. Development of an SPE Method Using Ionic Liquid-Based Monolithic Column for On-Line Cleanup of Human Plasma and Simultaneous Determination of Five Steroid Drugs. Chromatographia 81, 1391–1400 (2018). https://doi.org/10.1007/s10337-018-3579-0

Download citation

  • Received:

  • Revised:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s10337-018-3579-0

Keywords

Search

Navigation