Determination of the clean‐up efficiency of the solid‐phase extraction of rosemary extracts: Application of full‐factorial design in hyphenation with Gaussian peak fit function. Issue 3 (18th January 2018)

• Record Type: Journal Article
• Authors: Meischl, Florian; Kirchler, Christian Günter; Jäger, Michael Andreas; Huck, Christian Wolfgang; Rainer, Matthias
• Is Part Of: Journal of separation science. Volume 41:Issue 3(2018)
• Page Start: 704
• Page End: 712
• Publication Date: 2018-01-18
• Subjects: design of experiments -- extract purification -- peak quantification -- Rosmarinus officinalis -- sample preparation; Separation (Technology) -- Periodicals; Chromatographic analysis -- Periodicals; 543.089
• DOI: 10.1002/jssc.201701008
• Languages: English
• ISSNs: 1615-9306

Abstract

Abstract: We present a novel method for the quantitative determination of the clean‐up efficiency to provide a calculated parameter for peak purity through iterative fitting in conjunction with design of experiments. Rosemary extracts were used and analyzed before and after solid‐phase extraction using a self‐fabricated mixed‐mode sorbent based on poly( N ‐vinylimidazole/ethylene glycol dimethacrylate). Optimization was performed by variation of washing steps using a full three‐level factorial design and response surface methodology. Separation efficiency of rosmarinic acid from interfering compounds was calculated using an iterative fit of Gaussian‐like signals and quantifications were performed by the separate integration of the two interfering peak areas. Results and recoveries were analyzed using Design‐Expert® software and revealed significant differences between the washing steps. Optimized parameters were considered and used for all further experiments. Furthermore, the solid‐phase extraction procedure was tested and compared with commercial available sorbents. In contrast to generic protocols of the manufacturers, the optimized procedure showed excellent recoveries and clean‐up rates for the polymer with ion exchange properties. Finally, rosemary extracts from different manufacturing areas and application types were studied to verify the developed method for its applicability. The cleaned‐up extracts were analyzed by liquid chromatography with tandem mass spectrometry for detailed compound evaluation to exclude any interference from coeluting molecules.