Chromatographic fingerprint analysis—a rational approach for quality assessment of traditional Chinese herbal medicine (original) (raw)
Related papers
Comprehensive HPTLC fingerprinting as a tool for a simplified analysis of purity of ginkgo products
Journal of Ethnopharmacology
Ethnopharmacological relevance: Herbal medicinal products based on ginkgo leaf refined dry extract (GBE) are an European development from the Eastern Asia traditionally used species Ginkgo biloba L. Nowadays, ginkgo products have increased the presence in the market, mainly as dietary supplements. Its adulteration with rutin and quercetin or herbal extracts rich in these compounds is a common practice. Tests featuring assays and detection of adulterants need to be performed on top of other existent methods (e.g. identification test). This may increase the costs of evaluating the quality of ginkgo products. Aim of the study: To prove that comprehensive HPTLC fingerprinting can provide information beyond identification of ginkgo products, avoiding additional chromatographic tests for detection of adulterations. Materials and methods: The information contained in the fingerprint obtained by HPTLC analysis of flavonoids was used for identification and for detection of adulterants, as well as to verify the limits of rutin and quercetin, which are normally determined by HPLC and used for detection of adulterants. For this purpose, peak profiles were generated from HPTLC chromatogram images. USP-HPLC methods were used for quantification of total flavonoids and testing the limits of rutin and quercetin. HPLC data were used to support the validity of the HPTLC method. An additional reversed phase HPTLC method was developed as a possible confirmatory method for the quercetin limit test. Results: The proposed HPTLC method uses a particular sequence of detections, resulting in a number of images, which are later interpreted in a certain order. It is able to identify ginkgo products, to detect adulterants (rutin, quercetin, sophora fruit and flower bud, and buckwheat), and, using peak profiles generated from the chromatogram images prior to and after derivatisation, to evaluate the limits of rutin and quercetin. Forty-eight out of fifty-nine ginkgo dietary supplements analysed contained one or more adulterants. Furthermore, results of the HPTLC and HPLC limit tests for rutin and quercetin were in agreement in 98% of the cases. Finally, a decision tree showing the sequence of interpretation of the fingerprints obtained with the different detections after a single HPTLC analysis is included to help the analyst to evaluate whether samples have the correct identity and whether they contain or not adulterants. Arruda Frommenwiler et al. (revised)
Chromatography Research International
As traditional Chinese medicine (TCM) is gradually accepted by many countries, people pay much attention to the quality of herbal medicines. Because of the significant variation in active components in them, the quality control of herbal medicines is a very important issue. Nowadays, high-performance liquid chromatography (HPLC) fingerprint spectra (FPS) are widely used in identification and quality control of herbal medicines. This paper will analyze the methodology and their application in identifying and evaluating herbal medicines by means of HPLC FPS, which includes simple comparing, clustering, principal component analysis (PCA), and similarity analysis methods.
Fingerprint profile of Ginkgo biloba nutritional supplements by LC/ESI-MS/MS
Phytochemistry, 2008
Ginkgo biloba is one of the most popular herb nutrition supplements, with terpene lactones and flavonoids being the two major active components. A fingerprint profile method was developed using a capillary HPLC/MS method which can identify more than 70 components from the G. biloba product. The method allows the flavonoids and terpene lactones to be detected simultaneously and information of both the parent ion and its fragmentation can be obtained in just one HPLC/MS run. Targeted post-acquisition analysis allows mass spectrometric information regarding the identification of flavonoid components to be easily distinguished from other data, however the same approach for terpene lactones was less successful due to dimer formation and requires further development. The fingerprint profiles of five commercial G. biloba nutritional supplements were obtained and compared; variation of some components among the samples was observed and fortification could be detected. In the quality control analysis of the G. biloba product this method could be viewed as complementary to specific quantitative analysis of some bioactive components of the herb.
Journal of Chromatographic Science
Nowadays, increasingly more individuals turn to supplementation of the diet with herbal medicines and many such products are marketed lately. Thus the problem that this article focuses on is that these products are not subjected to rigorous quality control like synthetic drugs are, which rises a constant debate whether the supplements actually contain the herb or mixture of herbs that the manufacturer claims they do. As a solution, micellar electrokinetic chromatography and high performance liquid chromatography were investigated in order to fingerprint and authenticate herbal medicines. For this purpose, minimal sample pre-treatment was applied to several fruit based herbal medicines, which were compared with the ethanolic extract of the respective fruit. The holistic evaluation of the electropherograms and chromatograms was made by using appropriate chemometric tools, such as principal component analysis (PCA), cluster analysis and a combination of PCA and linear discriminant analysis (PCA-LDA). The results suggest that the developed method was able to successfully discriminate between different herbal medicines, based on their raw material content. Moreover, this simple and efficient methodology might also be used for routine screening and authenticity control of different products and could be implemented in any quality control laboratory.
Chemical Profiling of Ginseng Species and Ginseng Herbal Products Using UPLC/QTOF-MS
Journal of the Brazilian Chemical Society, 2016
The chemical profiles of four ginseng roots samples from three species of ginseng (Panax quinquefolius, Panax ginseng and Panax notoginseng) and two commercial ginseng products containing P. quinquefolius and red P. ginseng were compared using ultra-performance liquid chromatography coupled with quadrupole time of flight mass spectrometry (UPLC/QTOF-MS). Principal component analysis allowed a holistic approach in showing distinct chemical differences between the three ginseng species and correct classification of the two commercial products to their respective species. Further investigation of the chemical profile variations yielded ten main markers that were distinct for the three species. This study shows the potential of chemical profiling for the classification of complex natural product samples, such as ginseng, and application to commercial products sold in the market. This methodology can assist the industry in authenticating the various species of ginseng and providing a quick assessment of the quality of commercial ginseng products.
Analytical and Bioanalytical Chemistry, 2011
American ginseng (Panax quinquefolius) is one of the most commonly used herbal medicines in the world. Discriminating between P. quinquefolius grown in different countries is difficult using traditional quantitation methods. In this study, a liquid chromatographic mass spectrometry fingerprint combined with chemometric analysis was established to discriminate between American ginseng grown in the USA and China. Fifteen American ginseng samples grown in Wisconsin and 25 samples grown in China were used. The chromatographic fingerprints, representing the chemical compositions of the samples, made it possible to distinguish samples from the two locations. In addition, it was found that some ginsenosides varied widely from P. quinquefolius cultivated in these two countries. P. quinquefolius grown in the USA is higher in ginsenoside R c , ginsenoside R d , quinquenoside III/pseudo-ginsenoside RC 1 , malonyl ginsenoside R b1 , and ginsenoside R b2 , but lower in ginsenoside R b1 compared with P. quinquefolius grown in China. These ginsenosides may be responsible for the class separation seen using fingerprinting and chemometric approaches.
Detection of Adulterated Ginkgo biloba Supplements Using Chromatographic and Spectral Fingerprints
Journal of AOAC International, 2012
The fingerprints of 18 commercially available Ginkgo biloba supplements, 12 samples of raw G. biloba leaves, and three G. biloba standard reference materials from the National Institute of Standards and Technology were acquired directly (no chromatography) by UV spectrometry and after separation using HPLC with a diode array detector. The fingerprints consisted of the UV spectral images, the chromatographic images, and the areas of the 21 most prominent chromatographic peaks. Data were analyzed by principal component analysis and one-class soft independent modeling of class analogy (SIMCA). It was determined that three of the commercial products were adulterated with rutin, four with quercetin, and one with an unidentified flavonol glycoside. One-class SIMCA of the authentic products allowed the adulterated products to be easily distinguished using Q-residuals. Authentic supplements and raw leaf materials were easily distinguished. The finely powdered samples were also analyzed by near-IR (NIR) spectrometry. The authentic and adulterated products could not be distinguished by NIR spectrometry because of the excipients.
Journal of Food Science and Technology, 2015
Recently, the fingerprint approach using chromatography has become one of the most effective tools for quality assessment of herbal medicines and food supplements: due to the complexity of the chromatographic fingerprint and the irreproducibility of chromatographic instruments and experimental conditions, chemometric approach is employed to deal with the chromatographic fingerprint. The study was aimed at developing new analytical methods for the multivariate phytochemical fingerprinting of bioactive compounds in eight tree-species bud-preparations, commonly used in phytotherapy. Methods was used to identify and quantify the main bioactive compounds (polyphenols, organic acids and vitamins), and obtain a specific botanical profile in order to assess the contribution of each single bioactive class to the total bud preparation phytocomplex. A chemometric approach was used to distinguish among different genotypes assuring the identity, safety and quality of the botanical raw materials. The established protocol was simple, sensitive and reliable and it could be used for the evaluation and quality control of bud-extracts and natural food supplements: the proposed method was successfully applied to the characterization of commercial bud-preparations, demonstrating to be an effective tool for the fingerprinting of this plant material. The new approach developed in this study represents a good alternative for improving the classification results of herbal materials with complex chromatograms. It should be necessary to develop a Bmultivariate chromatographic fingerprint^, in order to differentiate the herbal preparations according to their genotype, avoiding substitutions, changes or adulterations with other species or synthetic drugs.
Journal of Biomedical Science, 2006
The quality of pharmaceutical products such as ginseng is important for ensuring consumer safety and efficacy. Ginseng is an expensive herb, and adulteration with other cheaper products may occur. Quality assurance of ginseng is needed since many of its commercial products now come in various formulations such as capsules, powder, softgels and tea. Thus traditional means of authentication via smell, taste or physical appearance are hardly reliable. Herbs like ginseng tend to exhibit characteristic infrared fingerprints due to their different chemical constituents. Here we report for the first time a rapid means of distinguishing American and Asian ginsengs from two morphological fakes-sawdust and Platycodon grandiflorum, via pattern differences and principal component analysis of their infrared spectra. Our results show that ginseng can be distinguished from both sawdust and Platycodon grandiflorum, hence there is a potential of using infrared spectroscopy as a novel analytical technique in the authentication of ginseng.
Analytical Letters, 2018
The commercial products of Panax ginseng have increasing market demand and high prices due to the pharmacological activities. To obtain high profits, P. ginseng may be adulterated with lower priced morphologically similar species such as Platycodon grandiflorum, Codonopsis lanceolata, and Pueraria lobata. This study was designed to validate accurate methods for the analysis of adulteration in P. ginseng products. High-performance liquid chromatography (HPLC) and ultraperformance liquid chromatography-diode array detectorelectrospray ionization-ion trap-time of flight-mass spectrometry (UPLC-DAD-ESI-IT-TOF-MS) were validated to analyze the raw plant materials, self-prepared formulations, and commercial products of P. ginseng, C. lanceolata, P. grandiflorum, and P. lobata. The developed analytical methods were confirmed by quality assurance parameters such as linearity, sensitivity, precision, and accuracy. Lobetyolin and ononin were identified as marker compounds by HPLC and confirmed by accurate mass measurement with ESI-IT-TOF-MS. HPLC analysis of self-prepared formulations indicated that by increasing the ratio of C. lanceolata, P. grandiflorum, and P. lobata in P. ginseng extracts, the peak area is increased at the same retention time. The limits of detection and quantification for lobetyolin and ononin were 0.098 and 0.171, and 0.108 and 0.726 mg/kg, respectively. Furthermore, the intraday precision (<1.0%) measurements confirmed that the developed analytical methods fulfill the required criteria for characterization of these products. The results demonstrated that the developed liquid chromatographic and mass spectrometric methods accurately characterized adulteration in P. ginseng commercial products.