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The identification of a specific toxic or regulated plant in herbal preparations or plant food supplements is a real challenge, since they are often powdered, mixed with other herbal or synthetic powders and compressed into tablets or capsules. The classical identification approaches based on micro- and macroscopy are therefore not possible anymore. In this paper infrared spectroscopy, combined with attenuated total reflectance was evaluated for the screening of plant based preparations for nine specific plants (five regulated and four common plants for herbal supplements). IR and NIR spectra were recorded for a series of self-made triturations of the targeted plants. After pretreatment of the spectral data chemometric classification techniques were applied to both data sets (IR and NIR) separately and the combination of both. The results show that the screening of herbal preparations or plant food supplements for specific plants, using infrared spectroscopy, is feasible. The best model was obtained with the Mid-IR data, using SIMCA as modelling technique. During validation of the model, using an external test set, 21 of 25 were correctly classified and six of the nine targeted plants showed no misclassifications for the selected test set. For the other three a success rate of 50% was obtained. Mid-IR combined with SIMCA can therefore be applied as a first step in the screening of unknown samples, before applying more sophisticated fingerprint approaches or identification tests described in several national and international pharmacopoeia. As a proof of concept five real suspicious samples were successfully screened for the targeted regulated plants. [ABSTRACT FROM AUTHOR]

Lonicera caerulea is a shrub native to the Northen Hemisphere, with its fruits having a long tradition of being used in traditional medicine. The flowers, although a potential source of diverse phenolic compounds have not been studied in terms of phenolic content. In this paper, a 2D LC heart-cutting system, operating in both on-line and off-line modes, was developed and successfully employed in identification and quantification of secondary metabolites in the flowers of L. caerulea . A total of 51 compounds have been resolved and identified as either flavonoids, phenolic acids or iridoids. Flavonoids were the dominating group of compounds, alongside substantial levels of both phenolic acids and iridoids. A comparison between three varieties of L. caerulea flowers revealed that ‘Wojtek’ contained markedly more flavonols and phenolic acids than the remaining two varieties, whereas iridoids were at similar levels. Heart-cutting 2D LC method used in this study offers a convenient approach and an effective tool for secondary metabolite analysis in L. caerulea flowers, and possibly other species from the genus. [ABSTRACT FROM AUTHOR]

African populations use traditional medicines in their initial attempt to treat a range of diseases. Nevertheless, accurate knowledge of the composition of these drugs remains a challenge in terms of ensuring the health of population and in order to advance towards improved traditional medicines (ITMs). In this paper chromatographic methods were developed for qualitative and quantitative analyses of a per os antimalarial ITM containing Garcinia kola. The identified analytical markers were used to establish TLC and HPLC fingerprints. G. kola seeds were analysed by HPLC to confirm the identity of the extract used by the Congolese manufacturer in the ITM. The main compounds (GB1, GB2, GB-1a and Kolaflavanone) were isolated by preparative TLC and identified by UPLC–MS and NMR. For the quantification of the major compound GB1, a simple and rapid experimental design was applied to develop an LC method, and then its validation was demonstrated using the total error strategy with the accuracy profile as a decision tool. The accurate results were observed within 0.14–0.45 mg/mL range of GB1 expressed as naringenin. The extracts used in several batches of the analysed oral solutions contained GB1 (expressed as naringenin) within 2.04–2.43%. Both the fingerprints and the validated LC-DAD were found suitable for the quality control of G. kola -based raw material and finished products, respectively. [ABSTRACT FROM AUTHOR]

Abstract: Acetophenones in Cynanchum species, especially cynandione A and its derivatives, whose utilization and toxicity in herbal drugs and folk medicines has caused great interest in the chemical investigation, have extensive biological activities. In this paper, a facile method based on high-performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry (HPLC-ESI-MS n ) was developed for the analysis of cynandione A derivatives in the roots of the Cynanchum wilfordii and C. auriculatum. ESI-MS/MS and ESI-MS n analysis of cynandiones A and B in negative ion mode were firstly performed employing two mass spectrometers each equipped with an ion-trap and a quadrupole time-of-flight (Q-TOF) mass analyzer. The results drawn from both instruments were similar to each other. Characteristic fragmentation pathways were proposed by comparing the spectra of two standards acquired in the experiments. The fragment ions at m/z 283 and 268 were obtained, and then were used as diagnostic ions to screen and identify cynandione A derivatives from the roots of above two species, together with an HPLC-MS n method. Total of 28 cynandione A derivatives comprising 4 reported and 24 novel components were identified or tentatively identified. Furthermore, breakdown curves were constructed to distinguish two types of isomers among these compounds. To our knowledge, this is the first report on characterization of acetophenones by HPLC-ESI-MS n , which allows a rapid and complete analysis of cynandione A derivatives in roots of Cynanchum species. [Copyright &y& Elsevier]