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

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.

Synthesis and Application of Histidine-Modified Poly(Glycidyl Methacrylate/Ethylene Glycol Dimethacrylate) Sorbent for Isolation of Caffeine from Black and Green Tea Samples

“…In this work, we focused on the development of a simple sample preparation procedure using SPE. Previous studies successfully showed that implication of weak anion-exchange-functionalized materials demonstrate high potential for isolation and clean-up of crude plant extracts [24,25]. After addition of HIS onto the present polymer backbone, the carboxy and imidazole functionalities remain free for interaction with molecules in solution.…”

“…These materials are typically crosslinked with DVB leading to a hydrophobic backbone. However, previous studies demonstrated that sorbents crosslinked with EGDMA as hydrophilic compound also exhibit excellent results for application with plant extracts [24,25]. The functional modifier HIS was chosen as it contains anionic (imidazole) and cationic (carboxylic acid) ion-exchange moieties.…”

The essential role of omni-capable research laboratories in advancing analytical spectroscopy

“…Strong emphasis is being put there on the method development and optimization. 23,25 What is rather unique, this unit puts a fair share of its attention into physicochemical and theoretical support of its analytical activity. 26,27 This is an essential aid securing a broader and deeper perspective, and providing an unmatched balance in the available scientific resource.…”

Design of experiments optimization application in physics: a case study of the damped driven pendulum experiment

“…Meischl et al have applied the full-factorial design in spelling with the Gaussian peak fitting function to determine the cleaning efficiency of solid-phase extraction of rosemary extracts [23]. Melo et al, the effect of Portland cement inclusions in hybrid glass fibre reinforced composites based on a full-factorial design [24].…”