DoE-assisted development and validation of a thin layer chromatography method for optimized separation of major cannabinoids in Cannabis sativa L. samples

As interest in the medical use of cannabis and cannabinoids rises, the need to establish appropriate quality specifications for them also becomes evident. Consequently, various methods applied to the analyses of cannabinoids in C. sativa have been reported. Among the chromatographic techniques used...

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Bibliographic Details
Published inJournal of liquid chromatography & related technologies Vol. 44; no. 15-16; pp. 809 - 819
Main Authors Ribeiro de Souza, Maíra, Limberger, Renata Pereira, Henriques, Amélia Teresinha
Format Journal Article
LanguageEnglish
Published Abingdon Taylor & Francis 02.10.2021
Taylor & Francis Ltd
Subjects
Analytical chemistry
Cannabinoids
Cannabis
Cannabis sativa
Chromatography
design of experiments
Optimization
Phase composition
quality control
Ruggedness
Selectivity
Thin layer chromatography
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Summary:As interest in the medical use of cannabis and cannabinoids rises, the need to establish appropriate quality specifications for them also becomes evident. Consequently, various methods applied to the analyses of cannabinoids in C. sativa have been reported. Among the chromatographic techniques used for this purpose, TLC stands out as a suitable alternative for fingerprint assessment. Nevertheless, structural similarity between cannabinoids imposes some analytical challenges. In this context, DoE-assisted optimization may favor achieving an adequate resolution between those analytes. Accordingly, this study aimed at developing and validating a TLC method for cannabinoid profile monitoring in C. sativa inflorescences by employing a DoE-driven strategy. A mixture design was applied to estimate the ideal mobile phase composition. Data analyses focused on maximizing resolutions between eight major cannabinoids and improving band distribution throughout the chromatogram. The overall quality of the chromatographic profiles after method optimization was satisfactory. Method validation covered selectivity, precision, and ruggedness assessment. The Youden design was applied for simultaneous analysis of five experimental factors. The proposed method was shown to be fit-for-purpose, allowing chemotype differentiation, in addition to being stability-indicating. Moreover, the results can support the definition of control strategies to ensure consistent achievement of the intended method's performance.
ISSN:1082-6076
1520-572X
DOI:10.1080/10826076.2022.2086566