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An ultrasound assisted extraction–solid‐phase extraction–ultra‐performance liquid chromatography combined strategy for atropine determination in Atropa belladonna leaves
Author(s) -
Koetz Mariana,
KleinJunior Luiz C.,
Santos Marí C.,
Silva Thamires A.,
Toson Natally S.B.,
Henriques Amélia T.
Publication year - 2021
Publication title -
biomedical chromatography
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.4
H-Index - 65
eISSN - 1099-0801
pISSN - 0269-3879
DOI - 10.1002/bmc.5053
Subject(s) - chromatography , atropa belladonna , extraction (chemistry) , chemistry , high performance liquid chromatography , solvent , atropine , solid phase extraction , anesthesia , traditional medicine , medicine , biochemistry
Atropine is an antimuscarinic alkaloid identified in Atropa belladonna . In pharmacopeias, percolation is standardized as an extraction method for A. belladonna leaves, along with liquid–liquid extraction as a cleanup procedure and titration as an analytical method for assaying the atropine in the leaves. In this study, a faster, solvent‐saving, and more reliable method for quality control of A. belladonna samples was developed. Ultrasound‐assisted extraction was proposed and optimized by fractional factorial design followed by Box–Behnken design. For modeling atropine content, the following optimal conditions were established: particle size, 180 μm; percentage methanol in water, 50%; volume of solvent, 15 ml; time of extraction, 60 min; and number of extractions, two. This led to a significant improvement in atropine extraction ( P < 0.001). For cleanup, solid‐phase extraction was used as an alternative to liquid–liquid extraction, giving similar results, with higher reproducibility. Finally, for the atropine assay, a UPLC method was validated as a substitute for the classic titration method. Taken together, the development of an ultrasound‐assisted extraction–solid‐phase extraction–UPLC approach allowed the determination of atropine content in A. belladonna leaves in a time‐ and solvent‐saving manner, with high reliability.