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Combination of On-Line Solid-Phase Extraction with LC-MS for the Determination of Potentially Hazardous Glycoalkaloids in Potato Products

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Abstract

A simple and rapid method for the determination of naturally occurring, potentially hazardous glycoalkaloids (GAs) in potatoes and their products has been developed. The procedure is based on the on-line solid-phase extraction of the acetic acid extracts from potato products and combined with liquid chromatography (LC)-mass spectrometry (MS) in a fully automated system (Symbiosis™, Spark Holland Instruments, Emmen, The Netherlands). As sorbent material HySphere™ 18HD was used for alkaloid enrichment. GAs were eluted with the LC gradient and directly analysed by MS. Detection of the analytes was achieved in the sensitive multiple reaction monitoring mode using two characteristic ions (m/z 98 as a qualifier for GAs and m/z 868.3 as a quantifier for α-solanine or m/z 852.4 for α-chaconine). Typical validation data for method precision (v k α-solanine = 5.3–6.5, v k α-chaconine = 3.4–15.4), accuracy (average recovery of α-solanine = 84%, average recovery of α-chaconine = 87%) and linearity over the range from 1 to 1,000 ng ml−1 (R 2 = 0.9915 for α-solanine, R 2 = 0.9939 for α-chaconine) with detection limits of 0.3 ng ml−1 for α-chaconine and 0.5 ng ml−1 for α-solanine were obtained. GA contents of commercial potato products were determined by the new on-line method and afterwards compared with those obtained with an established high-performance LC routine procedure. Better performance of the on-line procedure was obvious from the standard deviations of both methods. Other advantages included a strong reduction of overall analysis time, human intervention and solvent consumption as well as waste production. The time required for the on-line analysis was 5 min, which would allow processing of almost 100 samples in 8 h.

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Abbreviations

dw:

Dry weight

GA:

Glycoalkaloid

HPLC:

High-performance liquid chromatography

LC:

Liquid chromatography

LOD:

Limit of detection

LOQ:

Limit of quantification

MRM:

Multiple reaction monitoring

MS:

Mass spectrometry

R 2 :

Coefficient of determination

SPE:

Solid-phase extraction

v k :

Coefficient of variation

XLC:

Extraction-liquid chromatography

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Acknowledgements

We would like to thank the Landesstiftung Baden-Württemberg for financial support and Spark Holland Instruments, Emmen, The Netherlands, for their guidance in the XLC-MS method development.

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Authors and Affiliations

  1. Abteilung Biologie, Institut für Pharmazie und Molekulare Biotechnologie, Universität Heidelberg, Im Neuenheimer Feld 364, 69120, Heidelberg, Germany

    Melanie Distl & Michael Wink

  2. Spark Holland Instruments, P. De Keyserstraat 8, P. O. Box 288, 7800, AJ Emmen, The Netherlands

    Martin Sibum

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  1. Melanie Distl
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Correspondence to Michael Wink.

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Distl, M., Sibum, M. & Wink, M. Combination of On-Line Solid-Phase Extraction with LC-MS for the Determination of Potentially Hazardous Glycoalkaloids in Potato Products. Potato Res. 52, 39–56 (2009). https://doi.org/10.1007/s11540-008-9106-1

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