RESUMEN
In this paper, angelica broken wall powder(ABWP) was taken as the research object, HPLC fingerprint combined with multi-component determination(ferulic acid, senkyunolide I, coniferyl ferulate, ligustilide and 3-butylidenephthalide), physical fingerprint(D_(90), particle size distribution range, particle size distribution width, bulk density, tap density, inter-particle porosity, Carr index, specific surface area, pore volume, angle of repose, Hausner ratio, loss on drying and hygroscopicity)were used to characterize the quality attribute of ABWP; similarity analysis, cluster analysis, principal component analysis and orthogonal partial least squares discriminant analysis were conducted to construct the quality evaluation method of holographic analysis based on traditional Chinese medicine QbD "4 H mode", in order to evaluate the quality of ABWP from different sources and find out differentiated indicators. The quality evaluation method could be used for scientific, comprehensive evaluation of the quality attribute of ABWP, and the quality consistency evaluation of cell-wall-broken powder of different sources or different processes.It provides new ideas for quality control and research of ultrafine granular powders of traditional Chinese medicine.
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Angelica/química , Medicamentos Herbarios Chinos/análisis , Cromatografía Líquida de Alta Presión , Medicina Tradicional China , Polvos , Control de CalidadRESUMEN
BACKGROUND: Astragali Radix (AR) is a well-known Chinese herbal medicine. The quality of AR can be affected by many factors such as species, growth mode and production area, but there are still no chemical markers to distinguish it. PURPOSE: To explore chemical markers for improving the quality assessment of AR and discover chemical markers for identifying species, growth mode and production area of AR. METHODS: A highly sensitive, efficient and accurate method based on ultra-high performance liquid chromatography coupled to triple quadrupole mass spectrometry (UHPLC-QQQ-MS/MS) for simultaneous quantitative determination of 14 major chemical components (five flavonoids and nine triterpene saponins) in 94 batches of AR from China, Republic of Korea and Germany was developed for the first time. To explore chemical markers and assess changes in the contents of 14 compounds in the 94 batches of AR samples from different regions, hierarchical clustering analysis (HCA) and principal component analysis (PCA) were performed. RESULTS: Astragaloside III was not only an important chemical marker for distinguishing two species of AR, i.e.: Astragalus mongholicus and A. membranaceus, but also a potential chemical marker for the classification of cultivated and semi-wild AR. In addition, in the batches of cultivated AR, the content of isoastragaloside II and cyclocephaloside II were greater in batches from the region of Shaanxi Province than that of other Provinces in China, but the content of calycosin-7-O-ß-D-glucoside and astragaloside IV, which are the quality control markers of AR required by the Chinese Pharmacopoeia, were higher than that of other Provinces in China. In addition, the content of calycosin-7-O-ß-D-glucoside, ononin, calycosin and astragaloside I could be used to identify samples of AR collected from China, Republic of Korea and Germany. CONCLUSION: This UHPLC-QQQ-MS/MS method could be applied to the quantitative evaluation of AR and could be an important and meaningful reference to develop chemical markers for quality control of AR.
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Astragalus propinquus/química , Cromatografía Líquida de Alta Presión/métodos , Medicamentos Herbarios Chinos/análisis , Espectrometría de Masas en Tándem/métodos , Astragalus propinquus/crecimiento & desarrollo , China , Flavonoides/análisis , Alemania , Análisis de Componente Principal , Control de Calidad , Reproducibilidad de los Resultados , República de Corea , Saponinas/análisis , Triterpenos/análisisRESUMEN
Salvia miltiorrhiza (SM) is widely used to treat microcirculatory disturbance-related diseases; its lipophilic components play important roles in this application. Cryptotanshinone (CTS), tanshinone I (TSI) and tanshinone IIA (TSA) are the most widely-studied lipophilic ingredients, but low oral bioavailability limits their clinical application. It has been proven that micronization could improve the bioavailability of some drugs, so we've conducted this randomized study to investigate whether micronized granular powder (GP) of SM could improve the bioavailability of tanshinones compared with traditional decoction (TD). An oral dose of TD or GP of SM was administrated to subjects and blood samples were collected at predetermined time points. The plasma concentrations of tanshinones were detected by a validated method and pharmacokinetic parameters were calculated using a non-compartmental model. GP of SM resulted in a significant increase in mean maximum plasma concentration (C max ), elimination half-life and area under concentration-time curve (AUC) of tanshinones, with the plasma AUC of CTS, TSI and TSA in GP 5-184, 4-619 and 5-130 times higher than TD. In addition, the individual variances of C max and AUC were much lower after GP administration. Summarily, tanshinones in micronized GP of SM had higher oral bioavailability and lower individual variances, thus we speculate that it may indicate a better clinical efficacy and be a better choice than current treatments.
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Abietanos/farmacocinética , Composición de Medicamentos/métodos , Salvia miltiorrhiza/química , Abietanos/administración & dosificación , Administración Oral , Adulto , Disponibilidad Biológica , Femenino , Semivida , Voluntarios Sanos , Humanos , Masculino , Polvos , Adulto JovenRESUMEN
Near-infrared reflectance (NIR) spectroscopy combined with chemometric techniques was developed for classification and quantification of cheaper starches (corn and wheat starch) in ultrafine granular powder of Shanyao (UGPSY). By performing orthogonal partial least squares discrimination analysis (OPLS-DA), NIR could efficiently distinguish among authentic UGPSY and UGPSY adulterated with cornstarch and wheat starch. In addition, the starch content in adulterated UGPSY was determined by NIR coupled with an appropriate multivariate calibration method. Partial least squares (PLS), interval PLS (iPLS) and synergy interval PLS (siPLS) algorithms were performed comparatively to calibrate the regression model. Experimental results showed that the performance of the siPLS model is the best compared to PLS and iPLS. These results show that the combination of NIR spectroscopy and chemometric methods offers a simple, fast and reliable method for the classification and quantification of the ultrafine granular powder of the herb.
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Dioscorea/química , Contaminación de Alimentos/análisis , Espectroscopía Infrarroja Corta/métodos , Almidón/análisis , Triticum/química , Zea mays/química , Análisis de los Mínimos Cuadrados , Polvos/químicaRESUMEN
ETHNOPHARMACOLOGICAL RELEVANCE: Panax quinquefolius L (PQ), also known as American ginseng, has been used as a medicinal herb for thousands of years in the Far East, which was wildly used actively in healing the cardiovascular, endocrine and immune systems, in supporting chemoprevention of cancer. MATERIALS AND METHODS: An integrated, rapid, sensitive and reliable UHPLC-ESI-QQQ MS/MS method was validated and successfully applied in a pharmacokinetics study in which four representative ginsenosides were measured in beagle plasma following oral administration of Panax quinquefolius L (PQ) in the form of ultrafine granular powder, standard powder and an extract. RESULTS: Two paired ions ([M+Na](+) in the positive MS process, and two characteristic ions [Q3](+) in the positive MS/MS process) of the target compounds were optimized and selected for improved qualitative and quantitative analysis of ginsenosides in beagle plasma. The relative bioavailability of the target ginsenosides in these three formulations was measured by the pharmacokinetic parameters, including Cmax, Tmax, AUC0-∞ and so on. The ultrafine granular powder had the highest bioavailability, as well as the greatest extent of and fastest dissolution in vitro. CONCLUSION: Our results show that improved formulations of PQ could facilitate the dissolution and promote absorption of the important compounds it contains.
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Ginsenósidos/farmacocinética , Panax/química , Extractos Vegetales/farmacocinética , Animales , Área Bajo la Curva , Disponibilidad Biológica , Perros , Liberación de Fármacos , Ginsenósidos/sangre , Ginsenósidos/química , Semivida , Estructura Molecular , Extractos Vegetales/sangre , Extractos Vegetales/química , PolvosRESUMEN
This study aims to analyze and compare the effect of cell wall-broken decoction pieces, conventional decoction pieces and conventional powder of Rhodiolae Crenulatae Radix et Rhizoma on the intestinal flora of normal mice. The conventional bacterial culture and PCR-DGGE (polymerase chain reaction-denaturing gradient gel electrophoresis) were adopted for the mice after the oral administration for 14 days. According to the bacterial culture results, the 1/8 dose cell wall-broken decoction pieces group showed fewer Enterococcus and Escherichia coli bacillus but more Lactobacillus and Bifidobacterium than the conventional decoction pieces group and the traditional powder group (P <0.05). Meanwhile, on the basis of the PCR-DGGE results, the 1/8 dose cell wall-broken decoction pieces group revealed the highest Shannon-Wiener index (H) and species richness (S) among the seven groups, with extremely significant differences compared with the normal group (P <0.01), significant differences compared with the conventional decoction pieces group and the conventional powder group (P <0.05) and a high intra-group similarity. In conclusion, the long-term intake of 1/8 dose Rhodiolae Crenulatae Radix et Rhizoma cell wall-broken decoction pieces showed a certain effect in regulating intestinal tract by promoting the growth of Lactobacillus and Bifidobacterium. Furthermore, the intestinal flora community will become more stable.
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Intestinos/microbiología , Rhodiola , Animales , Bifidobacterium/efectos de los fármacos , Bifidobacterium/genética , Bifidobacterium/crecimiento & desarrollo , Pared Celular , Electroforesis en Gel de Gradiente Desnaturalizante , Lactobacillus/efectos de los fármacos , Lactobacillus/genética , Lactobacillus/crecimiento & desarrollo , Ratones , Ratones Endogámicos C57BL , Reacción en Cadena de la Polimerasa , RizomaRESUMEN
The dissolution of Panacis Quinquefolii Radix ultrafine granular powder and common powder, traditional pieces in water and simulated gastric juice in vitro was compared, and the effect of particles size of Panacis Quinquefolii Radix on the dissolution was studied. HPLC method was used for determination of five ginsenosides including Rg1, Re, Rb1, Rc and Rd from ultrafine granular powder and common powder, traditional pieces of Panacis Quinquefolii Radix at different points in time, furthermore, the dissolution curves of Panacis Quinquefolii Radix ultrafine granular powder and common powder, traditional pieces were obtained. The dissolution characteristics of the three Panacis Quinquefolii Radix forms were also compared in this study. According to the results, the dissolution rates of ginsenosides from ultrafine granular powder exceeded 90% of the total content with 5 min, significantly higher than that of the other two forms in water in vitro. At the same time, the dissolved amount of the ultrafine granular powder was fourteen percent higher than that of the traditional pieces and eight percent higher than that of the common powder. Under the condition of simulated gastric juice in vitro, the dissolution rates of ginsenosides from ultrafine granular powder were little lower than that of the other two, but the maximum dissolved amount of the former was fourteen percent higher than that of the common powder and five percent higher than that of the extracts. Therefore the conclusion is that micronization of Panacis Quinquefolii Radix contributed to dissolution of effective components.
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Ginsenósidos/química , Panax/química , Cromatografía Líquida de Alta Presión , Raíces de Plantas/química , Polvos , SolubilidadRESUMEN
Ultrafine powder and cell wall-broken powder of herbal medicine lack of the morphological characters and microscopic identification features. This makes it hard to identify herb's authenticity with traditional methods. We tested ITS2 sequence as DNA barcode in identification of herbal medicine in ultrafine powder and cell wall-broken powder in this study. We extracted genomic DNAs of 93 samples of 31 representative herbal medicines (28 species), which include whole plant, roots and bulbs, stems, leaves, flowers, fruits and seeds. The ITS2 sequences were amplified and sequenced bidirectionally. The ITS2 sequences were identified using Basic Local Alignment Search Tool (BLAST) method in the GenBank database and DNA barcoding system to identify the herbal medicine. The genetic distance was analyzed using the Kimura 2-parameter (K2P) model and the Neighbor-joining (NJ) phylogenetic tree was constructed using MEGA 6.0. The results showed that DNA can be extracted successfully from 93 samples and high quality ITS2 sequences can be amplified. All 31 herbal medicines can get correct identification via BLAST method. The ITS2 sequences of raw material medicines, ultrafine powder and cell wall-broken powder have same sequence in 26 herbal medicines, while the ITS2 sequences in other 5 herbal medicines exhibited variation. The maximum intraspecific genetic-distances of each species were all less than the minimum interspecific genetic distances. ITS2 sequences of each species are all converged to their standard DNA barcodes using NJ method. Therefore, using ITS2 barcode can accurately and effectively distinguish ultrafine powder and cell wall-broken powder of herbal medicine. It provides a new molecular method to identify ultrafine powder and cell wall-broken powder of herbal medicine in the quality control and market supervision.
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Código de Barras del ADN Taxonómico , Medicamentos Herbarios Chinos/análisis , Plantas Medicinales/clasificación , Pared Celular , ADN de Plantas/genética , ADN Espaciador Ribosómico/genética , Filogenia , Plantas Medicinales/genética , Polvos , Control de CalidadRESUMEN
OBJECTIVE: To establish the HPLC fingerprint of Clerodendrum lindleyi in order to provide the basis for its quality standard. METHODS: The chromatographic fingerprint was obtained with Angilent Zorbax C18 (250 mm x 4.6 mm, 5 µm) column and gradiently eluted with acetonitrile-0.1% phosphoric acid solution. The column temperature was maintained at 35 degrees C. The flow rate was 1.0 mL/min and the detection wavelength was 327 nm. RESULTS: HPLC fingerprint of Clerodendrum lindleyi was established and 21 common peaks from 11 batches of samples were found. CONCLUSION: The method has good precision, stability and repeatability, which can provide reliable basis for quality evaluation of Clerodendrum lindleyi.
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Cromatografía Líquida de Alta Presión , Clerodendrum/química , Medicamentos Herbarios Chinos/química , Medicamentos Herbarios Chinos/normas , Control de CalidadRESUMEN
OBJECTIVE: To develop an HPLC method for determination of emodin,chrysophanol and physcion from different medicinal parts of Berchemia lineata. METHODS: Samples were analyzed on Diamonsil ODS C18 (250 mm x 4. 6 mm,5 µm), with the mobile phase consisted of methanol-0. 20% phosphoric acid solution(74: 26). The flow rate was 1.0 mL/min,column temperature was set at 35 °C ,and detection UV wavelength was 254 nm. RESULTS: The linear range of emodin, chrysophanol and physcion was 0. 00201~ 0. 0804 µg,0. 0066~0. 264 µg and 0. 0124 ~0. 496 µg,with the average recovery was 100. 43% ,101. 29% and 98. 36% ,respectively. The content of total anthraquinones in root was higher than that in taten of Berchemia lineata. CONCLUSION: The method is simple,accurate and reliable for quality control of Berchemia lineata.
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Antraquinonas/análisis , Emodina/análogos & derivados , Emodina/análisis , Rhamnaceae/química , Cromatografía Líquida de Alta Presión , Raíces de Plantas , Control de CalidadRESUMEN
OBJECTIVE: To establish the HPLC fingerprint chromatograms of crude Notoginseng, cell wall-broken powder and cell wall-broken decoction pieces of Notoginseng and provide evidence for quality control of cell wall-broken decoction pieces of Notoginseng. METHODS: The HPLC procedure was performed on the chromatographic column of Hypersil ODS2, and the mobile phase was acetonitrile and water in gradient elution with the flow velocity of 1.0 mL/min. The detection wavelength was 203 nm and the column temperature was 25 degrees C. The chromatograms was analyzed with the software of "similarity evaluation system for chromatographic fingerprint of TCM". RESULTS: Eight common peaks were pinpointed from the chromatograms of different batches of crude Notoginseng, cell-broken powder and cell-broken decoction pieces, the similarities of the chromatograms were all larger than 0.9. CONCLUSION: The method of the HPLC fingerprint chromatogram is of good precision, reproducibility and stability,which is suitable for quality control of cell wall-broken decoction pieces of Notoginseng.
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Cromatografía Líquida de Alta Presión/métodos , Medicamentos Herbarios Chinos/química , Panax notoginseng/química , Saponinas/análisis , Raíces de Plantas/química , Polvos , Control de Calidad , Reproducibilidad de los Resultados , Rizoma/químicaRESUMEN
OBJECTIVE: To establish HPLC fingerprint of flavonoids and phenols of Dendrobium nobile. METHODS: Phenomenex prodigy ODS(3) C18 column (250 mm x 4.6 mm, 5 microm) was used with a mixture of acetonitrile-0.1% acetic acid as the mobile phase in a gradient mode, the column temperature was 25 degrees C, the flow rate was 1.0 mL/min, and the detection wavelength was 254 nm. RESULTS: The flavonoids and phenols of Dendrobium nobile were well separated, and 10 fingerprint peaks in common were confirmed. CONCLUSION: This method is simple, accurate with good reproducibility, and can be used specifically for the quality control of Dendrobium nobile.