ISSN print edition: 0366-6352 ISSN electronic edition: 1336-9075 Registr. No.: MK SR 9/7 Published monthly

Characterization and chemometric based optimization of bioactive metabolites in Hypoxis hemerocallidea with the aid of UPLC-QqQ-MS/MS

Mbuyelo Shikweni, Nikita Tawanda Tavengwa, and Tebogo Mphatlalala Mokgehle

Department of Chemistry, Faculty of Science, Engineering and Agriculture, Thohoyandou, South Africa

E-mail: tebogo.mokgehle@univen.ac.za

Received: 13 September 2023  Accepted: 22 November 2023

Abstract:

β-sitosterol and solasodine are major bioactive ingredients in Hypoxis hemerocallidea (H. hemerocallidea) with significant pharmacological properties. As a result, developing a simple and efficient extraction method for simultaneous extraction of both analytes is critical. The purpose of this study was to identify and separate β-sitosterol and solasodine from ethanolic extracts of H. hemerocallidea using a modified QuEChERS method and subsequent analysis via UPLC triple quadrupole mass spectrometry. Response surface methodology was carried out, which included numerical parameters such as ultrasonication time, centrifugation time, and ultrasonication power. The categorical factors included the type of salt used to facilitate extraction, which was (NH₄)₂SO₄ and Na₂SO₄. Fitting the response surface model to the experimental data produced a quadratic model with a good fit (R² = 0.9966 for solasodine and R² = 0.9857 for β-sitosterol). The optimum conditions for extraction of β-sitosterol and solasodine were an ultrasonication time of 30 min, ultrasonication power of 300 W and centrifugation time of 12 min. The generally higher concentrations of analytes obtained for (NH₄)₂SO₄ indicated that it had a superior salting-out ability compared to Na₂SO_4. In conclusion, for the first time, β-sitosterol and solasodine were simultaneously extracted using modified QuEChERS with good yields through the salting-out action of (NH₄)₂SO₄ in the presence of environmentally friendly solvents, ethanol and water. This modified QuEChERS technique can potentially be applied on a large scale as a sustainable and quick method for enrichment of therapeutic compounds from natural products.

Keywords: Modified QuEChERS; Solasodine; Hypoxis hemerocallidea; UPLC triple quadrupole mass spectrometry; β-sitosterol

Full paper is available at www.springerlink.com.

DOI: 10.1007/s11696-023-03232-1

Chemical Papers 78 (4) 2223–2233 (2024)