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ARS Home » Northeast Area » Beltsville, Maryland (BHNRC) » Beltsville Human Nutrition Research Center » Methods and Application of Food Composition Laboratory » Research » Publications at this Location » Publication #403082
Research Project: Advanced Technology for Rapid Comprehensive Analysis of the Chemical Components

Location: Methods and Application of Food Composition Laboratory

Title: Variation in botanical reference materials: similarity of actaea racemosa analyzed by flow injection mass spectrometry

Author
item Harnly, James - Jim
item UPTON, ROY - Us Pharmacipeia (USP)

Submitted to: Journal of AOAC International
Publication Type: Peer Reviewed Journal
Publication Acceptance Date: 12/13/2023
Publication Date: 12/23/2023
Citation: Harnly, J.M., Upton, R. 2023. Variation in botanical reference materials: similarity of actaea racemosa analyzed by flow injection mass spectrometry. Journal of AOAC International. 107(2): 332–344. https://doi.org/10.1093/jaoacint/qsad137.
DOI: https://doi.org/10.1093/jaoacint/qsad137

Interpretive Summary: The identity of botanical supplements is generally verified by comparing the chromatograms or spectra of an unknown material to those of botanical reference standards (BRMs). This comparison is difficult when the data for the reference standards are not consistent. This report presents a detailed study of the spectra of black cohosh (Actaea racemosa). The variance between 3 different reliable sources of BRMs is compared and various chemometric methods are used to improve the agreement. The difference between the vouchered samples is put in perspective by considering the systematic change in variance with genus, species, roots , and commercial supplements. Sometimes we must accept the reality that there is a lack of agreement and develop larger more comprehensive models in order to understand the limitations and also to search for more conserved sample components.

Technical Abstract: Botanical reference materials (BRMs) may be used as comparators for either determining identity (authenticity), quality, or purity of a plant material. Some highly characterized BRMs may account for species, cultivar, and year and location of harvest while more generic BRMs may have minimal characterization. All of these factors can result in variability in the chemical composition that may lead to statistically significant differences when applying chemometric profiling. Using flow injection mass spectrometry (FIMS), principal component analysis (PCA), and factorial multivariate analysis of variance (mANOVA), statistically significant (95% confidence limit, p=0.05) chemical composition differences were found between 3 genera (Actaea, Panax, and Ginkgo), 5 species of Actaea (A. racemosa, A. cimicifuga, A. dahurica, A. pachypoda, and A. rubra) root BRMs, 4 sources of A. racemosa root BRMs, and A. racemosa commercial roots and supplements. The variability of 6% of the BRM variables was found to be quantitatively conserved and reduced the compositional differences between the 4 sources of root BRMs. Compositional overlap of A. racemosa and other Actaea BRMs was influenced by variation in technical repeats, pre-processing methods, selection of variables, and selection of confidence limits. Frequency distribution plots provided the best means for understanding the impact of these variables on cross-validation and sensitivity and specificity. Sensitivity ranged from 94% to 97% and specificity ranged from 21% to 89% for the pre-processing protocols tested.