Multi-Detector Characterization of Grape Seed Extract to Enable in silico Safety Assessment

Abstract

Demands for increased analytical rigor have been growing within the botanical and dietary supplement industry due to concerns relative to safety, efficacy, and quality. Adulteration, ambiguous definitions, and insufficient perspective on safety are some of the major issues that arise when selecting a botanical extract. Herein, our comprehensive analytical approach is detailed for the selection of grape seed extracts. This approach provided characterization for the constituents above a threshold of toxicological concern by subjecting the extract to UHPLC-UV-CAD-HRMS and GC-FID & GC-HRMS. Thus, constituents within a wide range of volatility were evaluated. Furthermore, the extract was compared to authenticated botanical materials to confirm that no adulteration took place and was also compared to other grape seed extract sources to confirm that the material falls within the general profile. Finally, these data were cleared via an in silico safety assessment based on the list of constituents above the threshold of toxicological concern.

Incorporation of grape seed extract towards wound care product development

“…However, inherent biases of this detector can result in misrepresentation of the compounds that lack a chromophore (e.g., sugars, fatty acids, etc.) leading to biased quantitative information which can be overcome by the use of universal detectors, such as charged aerosol detector (CAD) and the incorporation of gas chromatography-flame ionization detector (GC-FID) and gas chromatography-high resolution mass spectrometry (GC-HRMS) to the ultrahigh-performance liquid chromatography-mass spectrometry (UHPLC-MS) analysis for toxicological safety assessment that would obviate the need for in vitro and in vivo safety analysis (Sica et al 2018).…”

The role of mass spectrometry and related techniques in the analysis of extractable and leachable chemicals

“…Ideally, reference standards would be available to confirm identification of all constituents and an in‐silico safety assessment of each chemical entity could be accurately addressed. Because this verification is not always possible, and many identifications cannot be compared against a reference standard, once a complete data set of information is generated on an unknown chemical, the constituent identifications are categorized at various levels of confidence (Jenke et al, ; USP 1663, 2015a; Sica et al, ). The level of confidence placed on an identification impacts the utility of the data.…”

“…The level of confidence placed on an identification impacts the utility of the data. Although the vocabulary and categories between companies and institutes might vary, identifications are typically categorized as confirmed , confident , or tentative (Jenke et al, ; USP 1663, 2015a; Baker and Regg, ; Sica et al, ). Confirmed identification indicates that the identity of an extractable chemical entity has been formally established through mass spectral and retention time match with an authentic reference compound.…”

“…Quantification with a more universal detector can further support the quantitative assessment. For instance, GC can employ a flame ionization detector (FID) and HPLC can use either an evaporative light scattering detector (ELSD) or a charged aerosol detector (CAD) (Górecki et al, ; Eom et al, ; Baker and Regg, ; Sica et al, ).…”

“…There has been a larger body of research in the pharmaceutical field that used the CAD to help quantify purity of drugs and degradants and was reviewed in 2012 (Almeling et al, ). HPLC‐CAD‐MS is a platform that has been used extensively to quantify and identify small molecule botanicals (Eom et al, ; Baker and Regg, ; Sica et al, ). The botanical safety approach uses the same TTC or SCT thresholds that are converted to an AET to draw the quantitative line for which all chemicals above need to be identified (Little et al, ).…”