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At-Line Monitoring of the Extraction Process of Rosmarini Folium via Wet Chemical Assays, UHPLC Analysis, and Newly Developed Near-Infrared Spectroscopic Analysis Methods

1
Institute of Analytical Chemistry and Radiochemistry, University of Innsbruck, Innrain 80/82, 6020 Innsbruck, Austria
2
School of Science and Technology, Kwansei Gakuin University, Gakuen, Sanda, Hyogo 669-1337, Japan
3
Michael Popp Research Institute for New Phyto Entities, University of Innsbruck, Mitterweg 24, 6020 Innsbruck, Austria
4
ADSI–Austrian Drug Screening Institute GmbH, Innrain 66a, 6020 Innsbruck, Austria
*
Author to whom correspondence should be addressed.
Authors contributed equally to this work.
Molecules 2019, 24(13), 2480; https://doi.org/10.3390/molecules24132480
Received: 13 June 2019 / Revised: 2 July 2019 / Accepted: 3 July 2019 / Published: 6 July 2019
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Abstract

The present study demonstrates the applicability of at-line monitoring of the extraction process of Rosmarinus officinalis L. leaves (Rosmarini folium) and the development of near-infrared (NIR) spectroscopic analysis methods. Therefore, whole dried Rosmarini folium samples were extracted by maceration with 70% (v/v) ethanol. For the experimental design three different specimen-taking plans were chosen. At first, monitoring was carried out using three common analytical methods: (a) total hydroxycinnamic derivatives according to the European Pharmacopoeia, (b) total phenolic content according to Folin–Ciocalteu, and (c) rosmarinic acid content measured by UHPLC-UV analysis. Precision validation of the wet chemical assays revealed a repeatability of (a) 0.12% relative standard deviation (RSD), (b) 1.1% RSD, and (c) 0.28% RSD, as well as an intermediate precision of (a) 4.1% RSD, (b) 1.3% RSD, and (c) 0.55% RSD. The collected extracts were analyzed with a NIR spectrometer using a temperature-controlled liquid attachment. Samples were measured in transmission mode with an optical path length of 1 mm. The combination of the recorded spectra and the previously obtained analytical reference values in conjunction with multivariate data analysis enabled the successful establishment of partial least squares regression (PLSR) models. Coefficients of determination (R2) were: (a) 0.94, (b) 0.96, and (c) 0.93 (obtained by test-set validation). Since Pearson correlation analysis revealed that the reference analyses correlated with each other just one of the PSLR models is required. Therefore, it is suggested that PLSR model (b) be used for monitoring the extraction process of Rosmarini folium. The application of NIR spectroscopy provides a fast and non-invasive alternative analysis method, which can subsequently be implemented for on- or in-line process control. View Full-Text
Keywords: ultra-high performance liquid chromatography; Folin–Ciocalteu; total hydroxycinnamic derivatives; phytoextraction; near-infrared spectroscopy ultra-high performance liquid chromatography; Folin–Ciocalteu; total hydroxycinnamic derivatives; phytoextraction; near-infrared spectroscopy
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This is an open access article distributed under the Creative Commons Attribution License which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited (CC BY 4.0).
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Delueg, S.; Kirchler, C.G.; Meischl, F.; Ozaki, Y.; Popp, M.A.; Bonn, G.K.; Huck, C.W. At-Line Monitoring of the Extraction Process of Rosmarini Folium via Wet Chemical Assays, UHPLC Analysis, and Newly Developed Near-Infrared Spectroscopic Analysis Methods. Molecules 2019, 24, 2480.

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