A high-performance thin-layer chromatographic (HPTLC) method for the analysis of the protostemonine from Stemona sessilifolia (Miq.) Miq. has been developed and validated. According to the HPTLC fingerprint, 12 common peaks were selected to evaluate the similarities among 10 batches of samples with RF values ranging from 0.02 to 0.95. Ten different batches of samples were stable and reliable in quality, all the similarities of which are more than 0.98. The results indicated that this method was sensitive and precise for the quality evaluation of S. sessilifolia samples.
Authors:Anna Hawrył, Ryszard Świeboda, Mirosław Hawrył, and Agata Ziobro
Ten methanolic extracts of selected Cirsium species were analyzed using two-dimensional thin-layer chromatography (2D-TLC) system with octadecyl reversed-phase (RP-18) chromatographic plate as the stationary phase and two eluents: nonaqueous, consisting of 2-butanone‒toluene‒acetic acid (4.5:5:0.5, v/v) used in the first direction of developing, and aqueous, consisting of methanol—water—formic acid (4:5:1, v/v) used in the second direction. The Naturstoff reagent was used for the derivatization of some phenolic compounds. Five selected standards were analyzed under the same chromatographic conditions, and their retention factor values were used for the confirmation of their presence on selected Cirsium chromatograms. Photographs of ten chromatograms were treated using the ImageJ program. 2D-TLC analysis was also performed to obtain the fingerprint chromatographic profiles of the studied methanolic extracts. The experimental data were objected to principal component analysis (PCA), and the PC2 vs. PC3 graphs were created. Based on the PCA results, the similarity between the selected Cirsium species was confirmed.
Authors:Petar M. Ristivojević and Gertrud E. Morlock
, J. Trifković , I. Vovk , D. Milojković-Opsenica , Comparative Study Of Different Approaches for Multivariate Image Analysis in HPTLC Fingerprinting of Plant Resin Extracts , 21st International Symposium on Separation Sciences
Authors:Jacques Pothier, Jacqueline Ragot, and Nicole Galand
The flavonoid and triterpenoid soyasaponin content of the aerial parts of
from four geographical origins of Africa (Ghana, Nigeria, Sierra Leone, and Togo) has been studied by planar chromatography, because the species is supposed to have hepato-protective activity. Comparative study of these compounds revealed the presence of flavonoids such as vitexine and isovitexine and soyasaponins such as soyasaponin I. The study proves the suitability of TLC analysis of soyasaponins for fingerprinting of this genus.
Authors:Fang Wang, Mei Meng, Li Chen, Xiaoyu Wang, and Qing Sun
The newly developed high-performance thin-layer chromatography (HPTLC) method allowed for the differentiation of QiYi capsules from 10 batches due to their characteristic fingerprints, proving to be a well-suited method for characterization and assignment of Traditional Chinese Medicine (TCM) preparation. The method was validated for repeatability, intra-precision, and inter-precision. The result was acceptable, with the reference of myotonin, because relative standard deviation (% RSD) was 3.9% in reproducibility test and less than 3.44% in inter- or intra-plate precisions. HPTLC fingerprinting of the extracts showed several peaks with different RF values. Eleven peaks were selected as the common peaks to evaluate the similarities of 10 different samples with RF values ranging from 0.10 to 0.87 according to fingerprint. The similarities of 10 batches of QiYi capsules were more than 0.940; it indicated that the different batches of QiYi capsules were stable and reliable in quality.
Authors:Mirosław A. Hawrył, Anna Hawrył, Ryszard Świeboda, Małgorzata Niemiec, and Monika Waksmundzka-Hajnos
Seven different Scutellaria species were analyzed using the extraction procedure (Soxhlet apparatus, dichloromethane, and methanol as solvents) and thin-layer chromatography method. Selected standards of flavonoids and phenolic acids (caffeic acid, chlorogenic acid, ferulic acid, baicalein, wogonin, baicalin, chrysin, quercetin, scutellarin, hesperetin, hesperidin, apigenin, luteolin, rutin, and kaempferol) were separated using silica gel thin-layer chromatography (TLC) plates with the mobile phase consisting of ethyl acetate—toluene—formic acid (5:4.9:0.1, v/v) for dichloromethane and methanolic extracts. Dichloromethane extracts were also developed using cyanopropyl-bonded silica gel with the following mobile phases: propan-2-ol—n-heptane—formic acid (5:4.9:0.1, v/v) and methanol—water—formic acid (6:3.9:0.1, v/v), and after drying, they were sprayed using the anisaldehyde reagent. In the case of methanolic extracts, the same non-aqueous eluent was used and the aqueous eluent consisting of methanol—water—formic acid (4:5.9:0.1, v/v). The presence of selected standards in Scutellaria species was confirmed. The similarities between the obtained fingerprint chromatograms were performed using chemometric methods, the similarity coefficients (Pearson’s correlation coefficient, determination coefficient, and congruence coefficient), distance indices (Euclidean distance, Manhattan distance, and Chebyshev’s distance), and multi-scale structural similarity (MS-SSIM).
Authors:Ningwei Lu, Wenxiang Zhang, Qiong An, Ning Li, and Yuming Dong
A two-dimensional thin-layer chromatographic fingerprint has been developed on a polyamide plate for the quality control of Helleborus thibetanus Franch. The investigated sample was separated by chloroform-ethyl acetate-methanol (3.0:8.0:4.4, v/v) in the first dimension and isooctane-n-propyl alcohol-water (10:2.5:1.0, v/v) adding 0.28 mol L−1 sodium dodecyl sulfate, a reversed micelle, in the second dimension. The plate was dried in the air at room temperature and examined in ultraviolet (UV) light at λ = 365 nm after development. The two developments were carried out over a distance of 70 mm. The two-dimensional thin-layer chromatographic method was validated in terms of repeatability, stability, and robustness. For fingerprint analysis, nine spots were identified as common spots. Statistical method (canonical correlation analysis) was first used to calculate the degree of similarity between the two-dimensional chromatograms. The proposed method was novel and accurate for the identification and quality evaluation of H. thibetanus Franch.
Authors:Anna Hawrył, Mirosław Hawrył, Ryszard Świeboda, and Monika Waksmundzka-Hajnos
Fourteen different Achillea species were extracted using the Soxhlet apparatus with dichloromethane and then methanol as solvents. The obtained dichloromethane and methanolic extracts were analyzed using thin-layer chromatography (TLC) and high-performance thin-layer chromatography (HPTLC) to obtain fingerprint profiles. The first chromatographic system consisted of silica gel as adsorbent, a mixture of toluene—ethyl acetate—formic acid (5:4.9:0.1, v/v) as the mobile phase and anisaldehyde as the derivatization reagent. The second adsorbent was cyano (CN) silica gel with non-aqueous (2-propanol and n-heptane [5:5, v/v], both for dichloromethane and methanolic extracts) and aqueous (methanol and water [6:4, v/v] for dichloromethane extracts and methanol and water [4:6, v/v] for methanolic extracts) mobile phases. Anisaldehyde (for dichloromethane extracts) and Naturstoff (for methanolic extracts) derivatization reagents were used. The obtained chromatograms were processed to obtain selected images using the ImageJ program. The similarity between the studied Achillea species was confirmed using the chemometric methods (principal component analysis [PCA], similarity, and distance measures).
Authors:He Zhang, Mei Meng, Li Chen, Fang Wang, Jing Zhang, Ying Jiang, and Wen Wang
The newly emerged chromatographic fngerprint analysis represents a rational approach assessment of Traditional Chinese Medicine (TCM) and its preparations. In the present paper, a quick and reliable analytical method was developed for the quality assessment of QiYi capsules (QY) using high-performance thin-layer chromatography (HPTLC) with the reference of Tripterygium wilfordii. The unique properties of the HPTLC fngerprint were validated by analyzing 10 batches of QY samples. The 9 common peaks of the HPTLC images of QY and the different RF and peak area ratios of the chemical distribution could directly discern the stability by comparison of 10 samples, and also, the 9 common peaks were selected to evaluate the similarities of QY; the similarities of 10 batches of QY were more than 0.960, which indicated a standardized consistency and reliable quality of QY. Therefore, the newly developed HPTLC fngerprint method provided an easy way for sample characterization and differentiation; it allowed for the quality assessment of QY capsules with the reference of T. wilfordii.