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. 2022 Aug 8:13:925298.
doi: 10.3389/fphar.2022.925298. eCollection 2022.

Investigation of market herbal products regulated under different categories: How can HPTLC help to detect quality problems?

Débora A Frommenwiler  1   2 , Eike Reich  1 , Maged H M Sharaf  3 , Salvador Cañigueral  2 , Christopher J Etheridge  4
Affiliations

Investigation of market herbal products regulated under different categories: How can HPTLC help to detect quality problems?

Débora A Frommenwiler et al. Front Pharmacol. .

Abstract

Background: Herbal products regulated under different categories were found to be of different quality. This has been demonstrated by the increasing number of reports on the quality of herbal products in the scientific literature. Proper identification is an effective way to address this concerning issue early on in a products' manufacturing process. Objectives: To assess the quality of milk thistle, coneflower and black cohosh herbal drugs, preparations and products commercialized under different regulatory categories, and to illustrate the usefulness of HPTLC as a tool for evaluating quality. Methods: HPTLC methods were adapted from the European Pharmacopeia's monographs for milk thistle fruits, black cohosh and purple coneflower. Additional detection modes beyond those described in the monographs were employed, and the entire HPTLC fingerprints were used for examination of identity and purity of the investigated samples. Results: All products regulated as Traditional Herbal Medicinal Products were shown to be of high quality: their fingerprints were consistent and without unexpected zones. A significant number of food supplements show quality issues (mainly adulterations): 52.4% of milk thistle, 33.3% of coneflower, and 45.5% of black cohosh products. The same was observed in 66.6% of black cohosh herbal drugs and preparations.

Keywords: HPTLC; THMP; black cohosh; coneflower; food supplement; milk thistle (Silybum marianum).

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Conflict of interest statement

The authors declare that the research was conducted in the absence of any commercial or financial relationships that could be construed as a potential conflict of interest.

Figures

FIGURE 1
FIGURE 1
Typical HPTLC fingerprints of milk thistle fruit, fruit extract, and herb prior to (right image) and after derivatization (left image). Left track in each image shows the chromatogram of the reference substances. Yellow arrows: blue zone characteristic of MT fruit, absent in MT fruit extract; Green arrow: chlorophyll zone characteristic of MT herb.
FIGURE 2
FIGURE 2
Fingerprints of the 31 milk thistle products in different detection modes, grouped by regulatory categories. Track A: silydianin, silychristin, taxifolin, and silybin in increasing R F values. Orange arrows: red zone due to chlorophyll detected in some products; red arrow: an unidentified yellow-white zone detected in some products.
FIGURE 3
FIGURE 3
Characteristic HPLTC fingerprints of standards (tracks A –E) and coneflower herbal drugs (tracks one–4): phenolic compounds (left image); alkylamides (after second heating step, right image). Yellow arrows: zones characteristic of Echinacea purpurea herb; black arrows: zones due to alkylamides of E. angustifolia root; purple arrow: zones characteristic of E. pallida root; blue arrow: zone due to alkylamides in E. purpurea root.
FIGURE 4
FIGURE 4
Alkylamide fingerprints of standards and Echinacea spp. products, in different detection modes. Tracks (A) echinacoside and cynarin, (B) chlorogenic and caffeic acids, (C) Ursolic acid and β-sitosterol and (D) dodeca-2E,4E,8Z,10E/Z-tetraenoic acid isobutylamide and dodec-2-ene-8,10-diynoic acid isobutylamide (with increasing R F); 1–23: ECH products 1–23.
FIGURE 5
FIGURE 5
Typical HPTLC fingerprints of Actaea racemosa and common adulterants prior to (top) and after derivatization (bottom). Left track in each image shows the chromatogram of the reference substances. Blue arrows: zones characteristic of A. podocarpa root; black arrow: zone due to actein in A. racemosa; purple arrow: zone due to 26-deoxyactein in A. racemosa.
FIGURE 6
FIGURE 6
Test for adulteration of Actaea racemosa with A. podocarpa, A. dahurica, and A. cimicifuga. Tracks 1, three and 5: A. racemosa; tracks 2, four and 6: A. racemosa mixed with 10% of A. podocarpa, 5% of A. dahurica and 5% of A. cimicifuga, respectively. Black arrow: zones characteristic of A. podocarpa root; orange arrows: zones characteristic of A. dahurica root; green arrow: zone due to cimifugin, characteristic of A. cimicifuga root.
FIGURE 7
FIGURE 7
HPTLC fingerprint of 11 black cohosh products and herbal drugs/herbal preparations. STD1: actein and isoferulic acid (increasing RF); STD2: cimifugin; RBCR: reference black cohosh root; RBCE: reference black cohosh root extract; 5% AD: Actaea racemosa mixed with 5% of A. dahurica; 5% AC: A. racemosa mixed with 5% of A. cimicifuga. Fingerprints (A,B) are used for identification of black cohosh root, while fingerprints (C,D) are used for detecting adulteration with A. dahurica and A. cimicifuga, respectively.
FIGURE 8
FIGURE 8
Summary of the quality of milk thistle products: number of samples/total products per category. THMP: Traditional Herbal Medicinal Product; FS: Food supplement.
FIGURE 9
FIGURE 9
Summary of the quality of coneflower products: number of samples/total products per category. THMP: Traditional Herbal Medicinal Product; FS: Food supplement.
FIGURE 10
FIGURE 10
Summary of the quality of black cohosh food supplement (FS) and herbal drugs and preparations (HDP): number of samples showing the concerned characteristic/total products per category. AC: Actaea cimicifuga; AD: A. dahurica; AR: A. racemosa.
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