[Evaluation of key production processes of Chan Taoren formula granules based on characteristic chromatogram and D-amygdalin transfer rate].

This study aimed to establish characteristic chromatogram and content determination method for Chan Taoren formula granules,evaluate the production processes of Chan Taoren formula granules based on the correlation of characteristic chromatogram and the transfer rate of D-amygdalin,and clarify the key control points. The optimized analytical method was carried out on a Waters CORTECS C18 column(4. 6 mm×150 mm,2. 7 µm) with acetonitrile-0. 1% phosphoric acid aqueous solution as the mobile phase at a flow rate of 0. 6 m L·min-1. The detection wavelength was 207 nm,and the column temperature was 20 ℃ ． As compared with the standard decoction of Chan Taoren,there were five characteristic peaks in the decoction pieces,extracts,concentrates,spray-dried powders and formula granules,basically consistent in relative retention time and peak pattern; in addition,the transfer rate of D-amygdalin from Chan Taoren pieces to the formula granules was within the transfer rate range of standard decoction. The average transfer rate of D-amygdalin was 56.65%,72.85%,94.58% and 99.29% respectively in the extraction,concentration,spray drying and granulation processes. Therefore,the factors affecting D-amygdalin in the extraction process were further studied. The results showed that D-amygdalin was easily converted to L-amygdalin in the water extraction process,leading to a low transfer rate of D-amygdalin in this process.D-amygdalin was unstable under alkaline conditions and prone to isomerization. Both liquid to solid ratio and extraction time had significant effects on the extraction rate of D-amygdalin. In this study,the key links in the production process of Chan Taoren formula granules was clarified based on the characteristic chromatogram and the quantity transmission of D-amygdalin,which provided a theoretical basis for production and quality control.

[Quality evaluation of Moutan Cortex Formula Granules].

A scientific and perfect quality evaluation system for Moutan Cortex Formula Granules was established,including content determination method,characteristic chromatogram method and mass spectrometry method. The content of paeoniflorin and paeonol in Moutan Cortex Formula Granules was determined by high performance liquid chromatography( HPLC),and the average content was 1. 72% and 1. 42%,respectively. The characteristic chromatogram was used to characterize Moutan Cortex Formula Granules,which contained 7 characteristic peaks,namely gallic acid,p-hydroxybenzoic acid,oxypaeoniflorin,paeoniflorin,tetragalloyl glucose,1,2,3,4,6-penta-O-galloyl-ß-D-glucose and paeonol. A total of 40 compounds in Moutan Cortex Formula Granules,including gallic acids,paeoniflorins,paeonols,flavonoids and benzoic acids,were identified by mass spectrometry. In this study,a variety of analytical methods were used to evaluate the quality system of Moutan Cortex Formula Granules,which could play a positive role in improving the level of quality evaluation and process quality control.

[Research on quality standards of standard decoction of Fructus Corni piece].

This study aims to develop the quality standards of Fructus Corni piece standard decoction. Morroniside and loganin were considered as index components. The content determination method of morroniside and loganin were developed. The fingerprint analysis method was also established. The standard decoctions of 15 batches of Fructus Corni pieces from Henan, Zhejiang, and Shaanxi were analyzed. The similarity values of fingerprint were all above 0.99. The transfer rates of morroniside were all higher than 100%. The quality evaluation indices of standard decoction were discussed. The transfer rate of an index component was not easy to be measured accurately and its concept was not rigorous. Therefore, index component yield was suggested as an evaluation index of standard decoction. Two methods for setting quality standards of standard decoctions, which were the ■ method and the ■ method, were compared. It was found that the standard range of ■ method was wider and more suitable for smaller sample size of standard decoction. The quality standards of Fructus Corni standard decoction were as follows, dry matter extraction ratio 37.48%-69.60%; morroniside yield 8.719-16.19 mg·g~(-1) piece; loganin yield 4.342-8.064 mg·g~(-1) piece.

Identification of xanthones from Swertia punicea using high-performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry.

RATIONALE: Swertia punicea Hemsl. (Gentianaceae) are used mainly for the treatment of acute bilious hepatitis, cholecystitis, fever, intoxification and jaundice in China, as a traditional Chinese folk medicine. Xanthones as the main chemical components of Swertia punicea have many possible pharmacological properties, such as hepatoprotective and anti-HIV. In order to obtain an overall picture of the xanthones of Swertia punicea, high-performance liquid chromatography diode-array detection/tandem mass spectrometry (HPLC/DAD-ESI-MS(n)) was applied to the structural characterization of xanthones in ethyl acetate and acetone extracts. METHODS: The ESI-MS fragmentation behaviors of xanthones were investigated based on the 17 reference xanthones and then applied to the structural characterization of xanthones in ethyl acetate and acetone extracts of Swertia punicea by HPLC/DAD-ESI-MS(n). RESULTS: The fragmentation rules of aglycone, C-glycosides, O-glycosides, and polyxanthones with different linkages were summarized. The observed fragmentation pathways were used successfully for the analysis of the xanthone constituents of Swertia punicea, and a total of 34 xanthones were identified, among which 16 compounds were new and one compound was reported from this species for the first time. CONCLUSIONS: The described methods were very valuable for the identification of xanthones, especially of the trace compounds, and therefore could be utilized for sensitive and rapid qualitative analysis of xanthones in Swertia punicea.

3-O-demethylswertipunicoside protects against oxidative toxicity in PC12 cells.

Xanthone compounds have been reported to inhibit cancer cell growth as well as possessing antioxidant properties. The xanthone compound 3-O-demethylswertipunicoside (3-ODS), extracted from Swertia punicea HEMSL, has not previously been demonstrated to have clear neuroprotective effects. In our study, the 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) cell death assay revealed that treatment of PC12 cells with 3-ODS ameliorated the decreased cell viability induced by exposure to 1-methyl-4-phenylpyridinium ion (MPP+), rotenone or H2O2. The acridine orange/ethidium bromide (AO/EB) apoptosis assay demonstrated a significant suppression of cell death in PC12 cells. by 3-ODS treatment. 3-ODS increased the protein expression of both tyrosine hydroxylase (TH) and DJ-1 expression in PC12 cells. The current study demonstrates that 3-ODS has potential neuroprotective effects mediated via the elevation of TH and DJ-1 protein levels.

Neuroprotective xanthone glycosides from Swertia punicea.

Two new dimeric xanthone O-glycosides, puniceasides A (1) and B (2), a new trimeric O-glycoside, puniceaside C (3), and two new trimeric C-glycosides, puniceasides D (4) and E (5), together with 12 known xanthones were isolated from the entire plant of Swertia punicea. The structures of 1-5 were determined by HRESIMS and NMR spectroscopic methods. Compounds 2, 6, and 7 exhibited potent neuroprotective activity against H(2)O(2)-induced PC12 cell damage.

Solvent effect in 1H NMR spectra of 3'-hydroxy-4'-methoxy isoflavonoids from Astragalus membranaceus var. mongholicus.

Four 3'-hydroxy-4'-methoxy-isoflavonoids: calycosin-7-O-beta-D-glucopyranoside (1), calycosin (2), pratensein-7-O-beta-D-glucopyranoside (3), and pratensein (4) were isolated from Astragalus membranaceus var. mongholicus, among which compound 4 was obtained from this plant for the first time. The solvent effect obscuring (1)H signal patterns of B ring of compounds 1-4 was reported to avoid mis-assignments. Previously reported NMR data of compounds 1 and 2 were corrected based on 1D and 2D NMR experiments.