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Analysis of Coumarin-Based Phototoxins in Citrus-Derived Essential Oils Using Liquid Chromatography-Mass Spectrometry

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Abstract

The occurrence of coumarin-based photoactive compounds in essential oils has been a concern due to the adverse health effects it has on human health. A fit-for-purpose analytical method for major coumarin-based phototoxins is critical to guarantee the essential oils product safety and compliance with the regulatory requirements. Herein, a liquid chromatography-mass spectrometry (LC–MS) analytical method was developed to identify and quantify 25 coumarin derivatives in essential oils. The sample preparation procedure was optimized to use selective solvent extraction to remove the limonene matrix interference. To achieve the optimal sensitivity and specificity, UHPLC column of biphenyl stationary phase was used for this analysis. An inter-laboratory validation study was conducted to evaluate the method performance. The limit of quantification (LOQ) for all target analytes was validated at 5 µg/g. Satisfactory recoveries were obtained for the majority of analytes in the range of 80–115%. Both the repeatability RSDr (within-laboratory) and reproducibility RSDR (between-laboratory) were < 10%. This method was demonstrated as applicable for the quality control testing of coumarin-based phototoxins in essential oils.

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Data Availability

The data available in this study are available in Table 1; Figs. 1, 2, 3, 4, 5, 6; and supplementary information. The datasets generated during this study are available from the corresponding author upon reasonable request.

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Acknowledgements

We kindly thank the colleagues from dōTERRA who contributed to this work, especially Nirmole Tambhar and Cecile Bascoul for the safety accessment of coumarins phototoxins, and Bryan Mauerman for providing the test samples. We also acknowledge Michael Scott, Sheila Stuligross, Megan Laryea-Akrong, Graham Curtin and Aaron Sorensen for their assistance.

Funding

No funding was received for this study.

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Authors and Affiliations

  1. dōTERRA International, 389 S 1300 W, Pleasant Grove, UT, 84062, USA

    Siheng Li, Radim Knob, Kent McConnell & Justin Barrett

  2. dōTERRA Global, Cork, Ireland

    Colleen Kelly

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  1. Siheng Li
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  2. Colleen Kelly
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  3. Radim Knob
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  4. Kent McConnell
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Contributions

S.L.: planning and performing the experiments, writing—original draft. C.K.: performing the experiments, and writing—review and editing. R.K.: writing—review and editing. K.M.: performing the experiments. J.B.: Conceptualization, resources, writing—review and editing.

Corresponding author

Correspondence to Siheng Li.

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Conflict of interest

Siheng Li declares he has no competing interests. Colleen Kelly declares she has no competing interests. Radim Knob declares he has no competing interests. Kent McConnell declares he has no competing interests. Justin Barrett declares he has no competing interests.

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This study does not involve human participants or animals.

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Li, S., Kelly, C., Knob, R. et al. Analysis of Coumarin-Based Phototoxins in Citrus-Derived Essential Oils Using Liquid Chromatography-Mass Spectrometry. Chromatographia 87, 59–69 (2024). https://doi.org/10.1007/s10337-023-04298-5

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