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Analysis of Crocetins and Safranal Variations in Saffron (Crocus sativus) Stigma Samples and Dietary Supplements Using HPLC/UHPLC-PDA-MS: Chemical Profiling and Chemometric Analysis Using LC-QToF

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Abstract

Saffron, the most expensive spice in the world, is comprised of the dried and dark red stigma of Crocus sativus L. flowers of the Iridaceae family. It is mainly used as a spice for imparting color, fragrance, and flavor to food but its medicinal and dyeing properties were also well known. In the USA, saffron products are used as dietary supplements for mood elevation, relaxation, weight loss, and to increase metabolism. The paper describes two analytical methods for the determination of crocetin esters, picrocrocin, safranal in saffron samples, and dietary supplements for inclusion in a monograph under development by the American Herbal Pharmacopoeia. Method validation showed satisfactory results in linearity, precision, and recovery. The content of picrocrocin, safranal, and crocetin esters ranged from 0.6–10.2%, 0.02–0.22%, and 2.8–25.6%, respectively, for thirty-seven stigma samples. Twenty-nine dietary supplements were analyzed. No saffron compounds were found in 16 (55%) of these products. Flower of Carthamus tinctorius and fruit of Gardenia jasminoides were the main adulterants detected in dietary supplements. Summarily, 60 compounds, including five standards were tentatively identified from saffron stigma, style, and petal samples using high-resolution mass spectrometry. Principle component analysis was used to discriminate between saffron stigma samples and dietary supplements. The results indicated that commercial products are of variable quality and the analytical method is suitable for quality assessment of a variety of both raw materials and finished dietary supplements.

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The datasets generated during the current study are available from the corresponding author on reasonable request and all analyzed data during this study are included in this article.

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Acknowledgements

This research is supported in part by “Science Based Authentication of Botanical Ingredients” funded by the Center for Food Safety and Applied Nutrition, US Food and Drug Administration grant number 5U01FD004246, and “Discovery & Development of Natural Products for Pharmaceutical & Agricultural Applications” funded by the United States Department of Agriculture, Agricultural Research Service, Specific Cooperative Agreement No. 58-6060-6-015.

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Correspondence to Bharathi Avula.

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Bharathi Avula declares that there is no conflict of interest. Kumar Katragunta declares that there is no conflict of interest. Yan-Hong Wang declares that there is no conflict of interest. Roy Upton declares that there is no conflict of interest. Ikhlas A. Khan declares that there is no conflict of interest.

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Avula, B., Katragunta, K., Wang, YH. et al. Analysis of Crocetins and Safranal Variations in Saffron (Crocus sativus) Stigma Samples and Dietary Supplements Using HPLC/UHPLC-PDA-MS: Chemical Profiling and Chemometric Analysis Using LC-QToF. Food Anal. Methods 15, 2238–2259 (2022). https://doi.org/10.1007/s12161-022-02268-5

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