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Determination of bitter orange alkaloids in dietary supplement Standard Reference Materials by liquid chromatography with atmospheric-pressure ionization mass spectrometry

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Abstract

A liquid chromatographic atmospheric-pressure ionization electrospray mass spectrometry (LC–API–ES–MS) method has been developed for the determination of five bitter orange alkaloids (synephrine, octopamine, n-methyltyramine, tyramine, and hordenine) in bitter orange-containing dietary supplement standard reference materials (SRMs). The materials represent a variety of natural, extracted, and processed sample matrices. Two extraction techniques were evaluated: pressurized-fluid extraction (PFE) and sonication extraction. The influence of different solvents, extraction temperatures, and pH were investigated for a plant material and a processed sample. The LC method uses a new approach for the separation of highly polar alkaloids. A fluorinated, silica-based stationary phase separated the five alkaloids and the internal standard terbutaline in less than 20 min. This method enabled the determination of the dominant alkaloid synephrine and other minor alkaloids in a variety of dietary supplement SRMs.

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Acknowledgement

The development of this suite of three bitter orange-containing SRMs is part of a collaborative effort with the National Institutes of Health’s Office of Dietary Supplements (NIH/ODS), and the Food and Drug Administration’s Center for Drug Evaluation and Research (FDA/CDER).

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  1. Karsten Putzbach

    Present address: RCC Ltd., Zelgliweg 1, CH-4452, Itingen, Switzerland

Authors and Affiliations

  1. Analytical Chemistry Division, National Institute of Standards and Technology, Gaithersburg, MD, 20899, USA

    Catherine A. Rimmer, Katherine E. Sharpless, Stephen A. Wise & Lane C. Sander

Authors
  1. Karsten Putzbach
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  2. Catherine A. Rimmer
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  3. Katherine E. Sharpless
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  4. Stephen A. Wise
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  5. Lane C. Sander
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Corresponding author

Correspondence to Lane C. Sander.

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Putzbach, K., Rimmer, C.A., Sharpless, K.E. et al. Determination of bitter orange alkaloids in dietary supplement Standard Reference Materials by liquid chromatography with atmospheric-pressure ionization mass spectrometry. Anal Bioanal Chem 389, 197–205 (2007). https://doi.org/10.1007/s00216-007-1409-6

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  • DOI: https://doi.org/10.1007/s00216-007-1409-6

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