Non-target bioanalytical eight-dimensional hyphenation including bioassay, heart-cut trapping, online desalting, orthogonal separations and mass spectrometry

Schreiner, Tamara; Morlock, Gertrud E.

doi:10.1016/j.chroma.2021.462154

Cited by 36 publications

(20 citation statements)

References 36 publications

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“…Hence, zones of interest were heart-cut eluted directly out of the bioassay plate and transferred through an online desalting device to RP-HPLC−DAD−HESI-MS. This reduced the interfering salts and nutrients from the bioassay, separated possibly coeluting substances via the orthogonal chromatographic system, and added value via spectral and mass spectrometric data ( Schreiner and Morlock, 2021 ). Through this straightforward comprehensive workflow, the 60 most bioactive compounds in the botanicals were assigned ( Table 2 ).…”

Section: Resultsmentioning

confidence: 99%

“…The MS was operated in polarity-switching mode, while the ESI probe was heated to 600°C and ESI source to 120°C. The sampling frequency was set to 5 Hz and cone voltage to ±10 V in both ionization modes ( Schreiner and Morlock, 2021 ). The MassLynx V4.2 software (Waters) was used to evaluate and process the data.…”

Section: Methodsmentioning

confidence: 99%

“…To overcome these limitations and expand the analytical toolbox, a high-throughput eight-dimensional (8D) hyphenat-ion was recently developed, and its proof of principle was shown for cinnamon samples detected with an antibacterial bioassay ( Schreiner and Morlock, 2021 ). It demonstrated the information gained by combining effect-directed assays (EDA) with normal-phase high-performance thin-layer chromatography including multi-imaging by ultraviolet, visible, and fluorescence light detection (NP-HPTLC−UV/Vis/FLD) ( Morlock, 2021 ).…”

Section: Introductionmentioning

confidence: 99%

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Is Our Natural Food Our Homeostasis? Array of a Thousand Effect-Directed Profiles of 68 Herbs and Spices

et al. 2021

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The beneficial effects of plant-rich diets and traditional medicines are increasingly recognized in the treatment of civilization diseases due to the abundance and diversity of bioactive substances therein. However, the important active portion of natural food or plant-based medicine is presently not under control. Hence, a paradigm shift from quality control based on marker compounds to effect-directed profiling is postulated. We investigated 68 powdered plant extracts (botanicals) which are added to food products in food industry. Among them are many plants that are used as traditional medicines, herbs and spices. A generic strategy was developed to evaluate the bioactivity profile of each botanical as completely as possible and to straightforwardly assign the most potent bioactive compounds. It is an 8-dimensional hyphenation of normal-phase high-performance thin-layer chromatography with multi-imaging by ultraviolet, visible and fluorescence light detection as well as effect-directed assay and heart-cut of the bioactive zone to orthogonal reversed-phase high-performance liquid chromato-graphy−photodiode array detection−heated electrospray ionization mass spectrometry. In the non-target, effect-directed screening via 16 different on-surface assays, we tentatively assigned more than 60 important bioactive compounds in the studied botanicals. These were antibacterials, estrogens, antiestrogens, androgens, and antiandrogens, as well as acetylcholinesterase, butyrylcholinesterase, α-amylase, α-glucosidase, β-glucosidase, β-glucuronidase, and tyrosinase inhibitors, which were on-surface heart-cut eluted from the bioautogram or enzyme inhibition autogram to the next dimension for further targeted characterization. This biological-physicochemical hyphenation is able to detect and control active mechanisms of traditional medicines or botanicals as well as the essentials of plant-based food. The array of 1,292 profiles (68 samples × 19 detections) showed the versatile bioactivity potential of natural food. It reveals how efficiently and powerful our natural food contributes to our homeostasis.

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Section: Resultsmentioning

confidence: 99%

Section: Methodsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Is Our Natural Food Our Homeostasis? Array of a Thousand Effect-Directed Profiles of 68 Herbs and Spices

et al. 2021

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“…A recently developed 8D hyphenation ( Schreiner and Morlock 2021 ) was alternatively used to further characterize the hormonal-effective compound zones. This hyphenation allowed eluting the bioactive zone from the bioautogram into the second separation and photodiode array (PDA) detection dimension (RP-HPLC-PDA-HESI-MS).…”

Section: Resultsmentioning

confidence: 99%

“…According to the latest workflow ( Schreiner and Morlock 2021 ) bioactive zones were eluted (TLC-MS Interface, CAMAG) with 10% aqueous methanol (MS-grade, Honeywell, Morristown, NJ, USA) provided by a standalone pump (515 HPLC pump, Waters, Eschborn, Germany) at a flow rate of 0.1 mL/min. The eluted zone was transferred through a biocompatible inline-filter (IDEX Health & Science, Oak Harbor, WA, USA) containing a PEEK frit (0.5 μm, Techlab, Braunschweig, Germany) to a two-position switching-valve (MXT-Series PD715-000, Rheodyne IDEX Health & Science), where the analytes were trapped on a defender guard/pre-column (Accucore RP-MS, 10 mm × 2.1 mm, 2.6 μm, Thermo Scientific, Bellefonte, PA, USA).…”

Section: Methodsmentioning

confidence: 99%

Evidence that Indo-Pacific bottlenose dolphins self-medicate with invertebrates in coral reefs

et al. 2022

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Sample preparation for planar chromatography

Poole

2023

J of Separation Science

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High‐performance thin‐layer chromatography has favorable properties for high‐throughput separations with a high matrix tolerance. Sample preparation, however, is sometimes required to control specific matrix interferences and to enhance the detectability of target compounds. Trends in contemporary applications have shifted from absorbance and fluorescence detection to methods employing bioassays and mass spectrometry. Traditional methods (shake‐flask, heat at reflux, Soxhlet, and hydrodistillation) are being challenged by automated instrumental approaches (ultrasound‐assisted and microwave‐assisted solvent extraction, pressurized liquid extraction, and supercritical fluid extraction) and the quick, easy cheap, efficient, rugged, and safe extraction method for faster and streamlined sample processing. Liquid‐liquid extraction remains the most widely used approach for sample clean‐up with increasing competition from solid‐phase extraction. On‐layer sample, clean‐up by planar solid‐phase extraction is increasingly used for complex samples and in combination with heart‐cut multimodal systems. The automated spray‐on sample applicator, the elution head interface, biological detection of target and non‐target compounds, and straightforward mass spectrometric detection are highlighted as the main factors directing current interest toward faster and simpler sample workflows, analysis of more complex samples, and the determination of minor contaminants requiring high concentration factors.

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Non-target bioanalytical eight-dimensional hyphenation including bioassay, heart-cut trapping, online desalting, orthogonal separations and mass spectrometry

Cited by 36 publications

References 36 publications

Is Our Natural Food Our Homeostasis? Array of a Thousand Effect-Directed Profiles of 68 Herbs and Spices

Is Our Natural Food Our Homeostasis? Array of a Thousand Effect-Directed Profiles of 68 Herbs and Spices

Evidence that Indo-Pacific bottlenose dolphins self-medicate with invertebrates in coral reefs

Sample preparation for planar chromatography

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