Abstract
Achyranthes bidentata Blume (AB) is a health food and a sulfur-free herbal medicine that is one of the most heavily sulfur-fumigated herbs in the marketplace. In this work, a comprehensive approach using ultra-performance liquid chromatography coupled with quadrupole time-of-flight-MS (UPLC-Q-TOF-MS) and multivariate statistical analysis was developed to identify characteristic sulfur-fumigation markers, elucidate chemical transformation mechanisms and characterize the degree of sulfur-fumigation of AB. Non-fumigated and sulfur-fumigated AB samples were compared by UPLC-Q-TOF-MS/MS analysis. Three triterpene saponins (Betavulgarosides II–IV) and two amides (Feruloyl-4-O-methyldopamine and Moupinamide) were identified as characteristic markers, which were positively correlated with two active AB components, namely oleanic acid and ferulic acid, respectively. Moreover, the extent of the sulfur-fumigation under different weight ratios of sulfur to herbal materials (1:20, 1:40, and 1:80) was analyzed based on chemical transformations and sulfur dioxide residues. Further verification showed that the ratio of 1:40 within 1 h was reasonable and efficient for herb quality preservation and assurance. This study provides a reliable sulfur-fumigation protocol for the quality control of AB and other herbs.
Highlights
Herbal materials have been handled during post-harvest by direct sun-drying or drying in the shade to obtain the dried root (China Pharmacopoeia [Part L], 2015)
Along with our previous study (Kang et al, 2017), the present study has identified five useful markers of sulfurfumigation in Achyranthes bidentata Blume (AB), which include three triterpene saponins (Betavulgarosides II–IV) and two amides (Feruloyl-4-Omethyldopamine and Moupinamide) using metabolomic combined with multivariate statistical analysis
We found that the chemical transformation of three triterpene saponin components declined after sulfur-fumigation, which were positively correlated with oleanic acid (OA), while the two amide components that accumulated after sulfur-fumigation were positively correlated with ferulic acid (FA)
Summary
Herbal materials have been handled during post-harvest by direct sun-drying or drying in the shade to obtain the dried root (China Pharmacopoeia [Part L], 2015). Some countries and regions of the Pharmacopeia, such as the China Pharmacopeia, the European Pharmacopeia, the United States Pharmacopeia, and the Korea Pharmacopeia, have developed standard limit values of sulfur dioxide residues (European Pharmacopoeia 8.0, 2014; Korean Pharmacopoeia XI, 2014; United States Pharmacopoeia, 2014; China Pharmacopoeia [Part L], 2015) This comprehensive indicator reflects the content of total sulfur dioxide or sulfurous acid, it indirectly reflects the loss of active components and health risk associated with sulfur-containing derivatives (Bai et al, 2015). This indicator does not evaluate the extent of the sulfur-fumigation of herbal medicines. It is our aim to further explore whether or not this practical protocol is reliable and applicable to all sulfur-fumigated herbs, especially those with no indigenous sulfur
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