Analytical and Bioanalytical Chemistry

, Volume 400, Issue 2, pp 395–401 | Cite as

SPE/RP-HPLC using C1 columns: an environmentally friendly alternative to conventional reverse-phase separations for quantitation of beta-carboline alkaloids in human serum samples

  • Víctor González-Ruiz
  • Ana I. Olives
  • M. Antonia Martín
Original Paper

Abstract

The analysis of beta-carboline alkaloids presents a renewed interest due to their biological relevance and their increasing popularity as recreational drugs. In the present work, a novel chromatographic reverse-phase high-performance liquid chromatography (RP-HPLC) method with fluorimetric detection has been applied to the determination of beta-carbolines spiked in human serum samples. The chromatographic procedure involves the use of less retentive, unusual C1 columns combined with hydro-alcoholic mobile phases and the use of beta-cyclodextrin or (2-hydroxypropyl)-beta-cyclodextrin as mobile-phase additives. The effective combination of C1 columns and the modified mobile phases with cyclodextrins leads to a considerable reduction in the organic proportion in the mobile phase (up to 50%) with good resolution and efficiency. Besides, the presence of cyclodextrins allows the use of ethanol, a green solvent, as the organic component in the mobile phase. Traditional RP-HPLC thus becomes an attractive eco-separation technique using conventional stationary phases under simple and user-friendly experimental conditions. Solid-phase extraction was employed as sample clean-up protocol with attractive features, i.e., a low consumption of organic solvents, time and step economy and diminished need for sample handling. The analytical procedure was completely validated showing satisfactory figures of merit. Limits of detection of 10−9–10−10 M can be achieved. The recoveries obtained for the total methodology (sample pre-treatment and chromatographic determination in the case of the mobile phases containing cyclodextrins) were very satisfactory (95–107%) as well as the intraday (2–3%) and interday precision values (3–7%). The use of 3-hydroxymethyl-beta-carboline as an internal standard allows the comparison of the goodness of response of the analytical methodology in the presence or absence of cyclodextrins.

Keywords

Cyclodextrins Eco-friendly mobile phases β-carboline derivatives HPLC 

Abbreviations

β-CD

β-Cyclodextrin

3HMBC

3-Hydroxymethyl-β-carboline

CDs

Cyclodextrins

HPβ-CD

2-Hydroxypropyl-β-cyclodextrin

HPLC

High-performance liquid chromatography

IS

Internal standard

MPA

Mobile-phase additives

QC

Quality control samples

RP

Reverse phase

SPE

Solid-phase extraction

Notes

Acknowledgments

Financial support from Ministerio de Ciencia e Innovación (SPAIN) through grant CTQ2009-11312 as well as from Grupos de investigación UCM grant 920234 is gratefully acknowledged. The authors are grateful to MEC for a FPU research fellowship for V. González-Ruiz.

Supplementary material

216_2010_4562_MOESM1_ESM.pdf (431 kb)
ESM 1(PDF 430 kb)

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Copyright information

© Springer-Verlag 2010

Authors and Affiliations

  • Víctor González-Ruiz
    • 1
  • Ana I. Olives
    • 1
  • M. Antonia Martín
    • 1
  1. 1.Sección Departamental de Química Analítica, Facultad de FarmaciaUniversidad Complutense de MadridMadridSpain

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