RESUMO
This study explored the preparation process of the placebo of Jiawei Ermiao Granules and evaluated the placebo effect, aiming to provide qualified placebo samples for clinical trials of Jiawei Ermiao Granules and a reference for the preparation and quality evaluation of placebos of traditional Chinese medicine granules. On the basis of the comprehensive analysis results of Jiawei Ermiao Granules, the orthogonal experiment was conducted to optimize the flavoring agents and colorants. After manual evaluation, the placebo formula was determined as dextrin 10 g, Codonopsis Radix extract 5.0 g, bitter melon extract 1.6 g, Mume Fructus extract 0.3 g, stevioside 0.1 g, sucrose octaacetate 0.004 g, indigo 0.004 g, lemon yellow 0.003 1 g, sunset yellow 0.001 8 g, bitter tea powder 0.001 8 g, caramel 0.001 3 g. Pilot trials were conducted on the placebo formula. The simulation effect of placebo was evaluated independently and comparatively, and the objectively evaluated by electronic nose and electronic tongue. The results showed that the independent manual evaluation of the placebo formula had higher error rate, and the placebo and Jiawei Ermiao Granules showed the similarity of 99.61% in the comparative manual evaluation. The smell similarity between the placebo and Jiawei Ermiao Granules was 99.19%, and the electronic tongue test showed little difference in the taste. In conclusion, the placebo prepared in this study shows a high similarity to Jiawei Ermiao Granules, which is not easy to break the blindness when being applied to clinical trials. This study provides a reference for the preparation and quality evaluation and promotes the large-scale production of placebos of traditional Chinese medicine granules, playing a role in improving the persuasiveness and acceptance of the efficacy of traditional Chinese medicines.
Assuntos
Medicamentos de Ervas Chinesas , Medicamentos de Ervas Chinesas/uso terapêutico , Medicina Tradicional Chinesa , PaladarRESUMO
BACKGROUND: Language deficits frequently occur during the prodromal stages of Alzheimer's disease (AD). However, the characteristics of linguistic impairment and its underlying mechanism(s) remain to be explored for the early diagnosis of AD. METHODS: The percentage of silence duration (PSD) of 324 subjects was analyzed, including patients with AD, amnestic mild cognitive impairment (aMCI), and normal controls (NC) recruited from the China multi-center cohort, and the diagnostic efficiency was replicated from the Pitt center cohort. Furthermore, the specific language network involved in the fragmented speech was analyzed using task-based functional magnetic resonance. RESULTS: In the China cohort, PSD increased significantly in aMCI and AD patients. The area under the curve of the receiver operating characteristic curves is 0.74, 0.84, and 0.80 in the classification of NC/aMCI, NC/AD, and NC/aMCI+AD. In the Pitt center cohort, PSD was verified as a reliable diagnosis biomarker to differentiate mild AD patients from NC. Next, in response to fluency tasks, clusters in the bilateral inferior frontal gyrus, precentral gyrus, left inferior temporal gyrus, and inferior parietal lobule deactivated markedly in the aMCI/AD group (cluster-level P < 0.05, family-wise error (FWE) corrected). In the patient group (AD+aMCI), higher activation level of the right pars triangularis was associated with higher PSD in in both semantic and phonemic tasks. CONCLUSIONS: PSD is a reliable diagnostic biomarker for the early stage of AD and aMCI. At as early as aMCI phase, the brain response to fluency tasks was inhibited markedly, partly explaining why PSD was elevated simultaneously.
Assuntos
Doença de Alzheimer , Disfunção Cognitiva , Humanos , Testes Neuropsicológicos , Estudos Transversais , Fala , Disfunção Cognitiva/diagnóstico , Doença de Alzheimer/diagnóstico , Doença de Alzheimer/patologia , Encéfalo/patologia , Imageamento por Ressonância Magnética , Estudos de Coortes , BiomarcadoresRESUMO
This study aimed to explore the triterpenic acid components in leaves of Ilex hainanensis. Alkaline water extraction, macroporous resin adsorption, and high performance liquid chromatography were used to separate and purify the triterpenic acid components in leaves of I. hainanensis. The physical and chemical property analysis, MS, NMR spectroscopy, and literature comparison were performed to identify the structures, and a new triterpene acid compound was discovered:(3S, 4R, 5R, 8R, 9R, 10R, 14S, 17S, 18S, 19R)-3,19-dihydroxyursa-12,20(30)-diene-24,28-dioic-acid, and named ilexhainanin F. In addition, according to its structural characteristics, the ~(19)F-NMR Mosher method was further employed to study its absolute configuration. By comparison of the ~(19)F-NMR chemical shifts of Mosher esters, it was determined that the absolute configuration of the 3-position chiral center of the compound was the S configuration.
Assuntos
Ilex , Triterpenos , Cromatografia Líquida de Alta Pressão/métodos , Ilex/química , Espectroscopia de Ressonância Magnética , Estrutura Molecular , Folhas de Planta/química , Triterpenos/análiseRESUMO
This study employed Box-Behnken design combined with flux attenuation to explore the nanofiltration conditions for separation of alcohol precipitation liquid during the preparation of Reduning Injection and discussed the applicability of nanofiltration in the separation of the liquid with high-concentration ethanol. The effects of nanofiltration molecular weight cut-off(MWCO) and pH on the rejection of chlorogenic acid, 3,5-dicaffeoylquinic acid, and 4,5-dicaffeoylquinic acid were consistent with the principles of pore size sieving and charge effect, respectively. The rejection of the three phenolic acids was reduced by concentration polarization effect caused by trans-membrane pressure(TMP). The swelling of membrane surface decreased the pore size and membrane flux for effective separation. Chlorogenic acid and 4,5-dicaffeoylquinic acid were more sensitive to pH and ethanol concentration than 3,5-dicaffeoylquinic acid. A certain correlation existed between the compound structure and the separation factors of nanofiltration, and the separation rules were associated with the comprehensive effect of charge effect, pore size sieving, concentration polarization, steric hindrance and so on.
Assuntos
Ácido Clorogênico , Medicamentos de Ervas Chinesas , Medicamentos de Ervas Chinesas/química , Etanol , InjeçõesRESUMO
Alzheimer's disease (AD) is a leading cause of dementia. However, the mechanisms responsible for development of AD, especially for the sporadic variant, are still not clear. In our previous study, we discovered that a small noncoding RNA (miR-188-3p) targeting ß-site amyloid precursor protein cleaving enzyme (BACE)-1, a key enzyme responsible for Aß formation, plays an important role in the development of neuropathology in AD. In the present study, we identified that miR-338-5p, a new miRNA that also targets BACE1, contributes to AD neuropathology. We observed that expression of miR-338-5p was significantly down-regulated in the hippocampus of patients with AD and 5XFAD transgenic (TG) mice, an animal model of AD. Overexpression of miR-338-5p in the hippocampus of TG mice reduced BACE1 expression, Aß formation, and neuroinflammation. Overexpression of miR-338-5p functionally prevented impairments in long-term synaptic plasticity, learning ability, and memory retention in TG mice. In addition, we provide evidence that down-regulated expression of miR-338-5p in AD is regulated through the NF-κB signaling pathway. Our results suggest that down-regulated expression of miR-338-5p plays an important role in the development of AD.-Qian, Q., Zhang, J., He, F.-P., Bao, W.-X., Zheng, T.-T., Zhou, D.-M., Pan, H.-Y., Zhang, H., Zhang, X.-Q., He, X., Sun, B.-G., Luo, B.-Y., Chen, C., Peng, G.-P. Down-regulated expression of microRNA-338-5p contributes to neuropathology in Alzheimer's disease.
Assuntos
Doença de Alzheimer/genética , Hipocampo/metabolismo , MicroRNAs/fisiologia , Regiões 3' não Traduzidas , Doença de Alzheimer/metabolismo , Secretases da Proteína Precursora do Amiloide/biossíntese , Secretases da Proteína Precursora do Amiloide/genética , Peptídeos beta-Amiloides/metabolismo , Animais , Ácido Aspártico Endopeptidases/biossíntese , Ácido Aspártico Endopeptidases/genética , Células Cultivadas , Modelos Animais de Doenças , Regulação para Baixo , Humanos , Inflamação , Masculino , Aprendizagem em Labirinto , Transtornos da Memória/genética , Transtornos da Memória/prevenção & controle , Camundongos , Camundongos Transgênicos , MicroRNAs/biossíntese , MicroRNAs/genética , NF-kappa B/fisiologia , Plasticidade Neuronal , Neurônios/metabolismo , Fragmentos de Peptídeos/metabolismo , Cultura Primária de Células , Proteínas Recombinantes/metabolismoRESUMO
BACKGROUND: The statistical association between a short-term rise in low-density lipoprotein cholesterol (LDL-C) levels and the short-term outcome of acute ischemic stroke remains unknown. We aimed to evaluate the association in acute ischemic stroke patients during hospitalization. METHODS: Patients with acute ischemic stroke who received statin at discharge were enrolled in this multicenter registry study. LDL-C values were measured on the first day after admission and on the day before discharge to determine the rise in LDL-C levels. Poor outcome was defined as a modified Ranking Scale score ≥2 at discharge. The National Institutes of Health Stroke Scale increase from admission to discharge by 2 points was defined as clinical deterioration. Logistic regression analyses were used to analyze the relationship between LDL-C rise during hospitalization and poor outcome at discharge. Variables that were significantly different between the LDL-C rise and LDL-C fall groups were considered in adjustment for confounding variables in model 1. Age, sex, and those variables in model 1 were considered in adjustment for confounding variables in model 2. RESULTS: Among the 676 patients, 110 (16.3%) showed a rise in LDL-C levels during hospitalization. Multivariate analyses showed that LDL-C at admission <1.6 mmol/L was significantly correlated with LDL-C rise during hospitalization (p < 0.001). There were significantly more patients with a poor outcome in the "LDL-C rise" group than in the "LDL-fall" group (p = 0.002). Multiple models consistently showed that LDL-C rise increased the risk of a poor outcome at discharge in model 1 (OR [95% CI] 1.351 [1.059-1.723], p = 0.016) and model 2 (OR [95% CI] 1.370 [1.071-1.751], p = 0.012). LDL-C rise also increased the risk of clinical deterioration, although its p value only was 0.043 in model 1 and 0.048 in model 2. CONCLUSIONS: Rise in LDL-C during hospitalization from acute ischemic stroke is an independent predictor of poor outcome at discharge. In particular, patients with lower LDL-C values at admission are a higher at risk, and LDL-C in these patients should thus be monitored while in hospital.
Assuntos
Isquemia Encefálica/terapia , LDL-Colesterol/sangue , Inibidores de Hidroximetilglutaril-CoA Redutases/uso terapêutico , Alta do Paciente , Acidente Vascular Cerebral/terapia , Idoso , Biomarcadores/sangue , Isquemia Encefálica/sangue , Isquemia Encefálica/diagnóstico , Isquemia Encefálica/fisiopatologia , China , Avaliação da Deficiência , Feminino , Humanos , Masculino , Pessoa de Meia-Idade , Admissão do Paciente , Sistema de Registros , Fatores de Risco , Acidente Vascular Cerebral/sangue , Acidente Vascular Cerebral/diagnóstico , Acidente Vascular Cerebral/fisiopatologia , Fatores de Tempo , Resultado do Tratamento , Regulação para CimaRESUMO
Safflower has both medicinal and edible values but research on its nutrient composition is still lacking. This study was established for the quantitative determination of 28 nucleosides, nucleobases, and amino acids based on the ultra-performance liquid chromatography coupled with triple-quadrupole linear ion-trap tandem mass spectrometry. Analysis of 30 batches of safflower from different producing areas indicated that the contents of l-proline, l-asparagine, l(+)-arginine, l-serine, l-histidine, uracil, guanosine, and uridine was high in safflower. Principle component analysis and cluster analysis found that samples from different regions could be distinguished well, and samples from the same area could be clustered into one class, different geographical environments may cause the differences of nucleosides, nucleobases, and amino acids in safflower. The analysis of principal component analysis, cluster analysis, and counter propagation artificial neural network show similar results. Then the content of nucleosides, nucleobases, and essential amino acids were compared, and found that the content in safflower from Gansu was higher than those from other regions, and there was a little difference between the samples from Xinjiang, Sichuan, and Yunnan. This research revealed the composition of nucleosides, nucleobases, and amino acids in safflower, and provided a theoretical basis for utilization of safflower.
Assuntos
Aminoácidos/análise , Carthamus tinctorius/química , Nucleosídeos/análise , Cromatografia Líquida de Alta Pressão , Análise por Conglomerados , Análise de Componente Principal , Espectrometria de Massas em TandemRESUMO
This work is to establish the fingerprint of Astragalus membranaceus var. mongholicus by HPLC-ELSD method, and to analyze the simulated wildness degree of A. membranaceus var. mongholicus in the genuine region of Inner Mongolia, Ningxia and Gansu. Compared with wild A. membranaceus var. mongholicus, the quality differences of A. membranaceus var. mongholicus in the genuine region were analyzed by identification of chromatographic peaks and similarity evaluation, cluster analysis(CA), principal components analysis(PCA) and orthogonal partial least squares discriminant analysis(OPLS-DA). HPLC fingerprints of A. membranaceus var. mongholicus in different genuine regions are established. The qualitative analysis of mass spectrometry identified 18 components. The similarity evaluation shows that the similarity of 32 batches of A. membranaceus var. mongholicus samples was 0.688-0.993. Among them, the similarity of samples in Shanxi, Inner Mongolia, Ningxia is 0.688-0.993, 0.835-0.989, 0.934-0.988, respectively and the similarity of samples in Gansu is 0.729-0.876 except No. 25 sample. The results of CA show that the samples of A. membranaceus var. mongholicus can be grouped into four categories according to the production area except the No. 11 and No. 25 samples. The results of PCA indicate that 32 batches of A. membranaceus var. mongholicus samples can be clustered according to quality and origin, and the quality of A. membranaceus var. mongholicus in Inner Mongolia is the closest to the wild breed. The results of OPLS-DA indicate that there are six components that can distinguish the wild and domestic A. membranaceus var. mongholicus, which are malonylastragaloside â , astragaloside â , calycosin-7-O-ß-D-glycoside-6â³-O-malonate, calycosin-7-O-ß-D-glycoside, formononetin-7-O-ß-D-glycoside-6â³-O-malonate, and astrapterocarpan-3-O-ß-D-glycoside-6â³-O-malonate. The established method can be used to analyze differences between A. membranaceus var. mongholicus origin and planting environment, and can provide references for the protection and replacement of wild A. membranaceus var. mongholicus resources, and the cultivation, processing and production of A. membranaceus var. mongholicus.
Assuntos
Astragalus propinquus , ChinaRESUMO
Poria cocos (P. cocos) polysaccharides (PCPs) are used to improve immunity and possess antitumor activities. We compared three cultivars of P. cocos (5.78, XJ 28 and JHYH) PCP contents. Then we determined that malZ, galA, SORD, gnl and bglX are key enzymes within the PCP biosynthetic pathway by using HiSeq2500 transcriptome and qRT-PCR validation. Our results provide more detailed information about the PCP biosynthesis pathway at the molecular level in P. cocos and establish the functions for the molecular breeding to produce polysaccharides in general for therapeutic use in Chinese medicinal plants.
Assuntos
Polissacarídeos Fúngicos/metabolismo , Transcriptoma , Wolfiporia/metabolismo , Polissacarídeos Fúngicos/genética , Regulação Fúngica da Expressão Gênica , Wolfiporia/genéticaRESUMO
In the present study, a new strategy including the combination of external appearance, chemical detection, and biological analysis was proposed for the comprehensive evaluation of safflowers in different producing areas. Firstly, 40 batches of safflower samples were classified into class I and II based on color measurements and K-means clustering analysis. Secondly, a rapid and sensitive analytical method was developed for simultaneous quantification of 16 chromaticity-related characteristic components (including characteristic components hydroxysafflor yellow A, anhydrosafflor yellow B, safflomin C, and another 13 flavonoid glycosides) in safflowers by ultra-performance liquid chromatography coupled with triple-quadrupole linear ion-trap tandem mass spectrometry (UPLC-QTRAP®/MS2). The results of the quantification indicate that hydroxysafflor yellow A, anhydrosafflor yellow B, kaempferol, quercetin, and safflomin C had significant differences between the two types of safflower, and class I of safflower had a higher content of hydroxysafflor yellow A, anhydrosafflor yellow B, and safflomin C as the main anti-thrombotic components in safflower. Thirdly, chemometrics methods were employed to illustrate the relationship in multivariate data of color measurements and chromaticity-related characteristic components. As a result, kaempferol-3-O-rutinoside and 6-hydroxykaempferol-3-O-ß-d-glucoside were strongly associated with the color indicators. Finally, anti-thrombotic analysis was used to evaluate activity and verify the suitability of the classification basis of safflower based on the color measurements. It was shown that brighter, redder, yellower, more orange-yellow, and more vivid safflowers divided into class I had a higher content of characteristic components and better anti-thrombotic activity. In summary, the presented strategy has potential for quality evaluation of other flower medicinal materials.
Assuntos
Carthamus tinctorius/química , Fenômenos Químicos , Compostos Fitoquímicos/química , Compostos Fitoquímicos/farmacologia , Animais , Carthamus tinctorius/classificação , Cromatografia Líquida de Alta Pressão , Fibrinolíticos/química , Fibrinolíticos/farmacologia , Geografia , Espectrometria de Massas em Tandem , Peixe-ZebraRESUMO
Based on the molecular sieving and solution-diffusion effect in nanofiltration separation, the correlation between initial concentration and mass transfer coefficient of three typical phenolic acids from Salvia miltiorrhiza was fitted to analyze the relationship among mass transfer coefficient, molecular weight and concentration. The experiment showed a linear relationship between operation pressure and membrane flux. Meanwhile, the membrane flux was gradually decayed with the increase of solute concentration. On the basis of the molecular sieving and solution-diffusion effect, the mass transfer coefficient and initial concentration of three phenolic acids showed a power function relationship, and the regression coefficients were all greater than 0.9. The mass transfer coefficient and molecular weight of three phenolic acids were negatively correlated with each other, and the order from high to low is protocatechualdehyde >rosmarinic acid> salvianolic acid B. The separation mechanism of nanofiltration for phenolic acids was further clarified through the analysis of the correlation of molecular weight and nanofiltration mass transfer coefficient. The findings provide references for nanofiltration separation, especially for traditional Chinese medicine with phenolic acids.
Assuntos
Hidroxibenzoatos/análise , Salvia miltiorrhiza/química , Peso MolecularRESUMO
Based on the nanofiltration mass transfer model, the enhanced separation behavior of ephedrine in organic solution was studied. In the experiment, the sensitive region of ethanol concentration and pH on the rejection of ephedrine was screened out by Box-Behnken central composite experiment design. Furthermore, to analyze the separation regularity of ephedrine and organic solution, the correlation between mass transfer coefficient and concentration of organic solvent was fitted with the changed organic solution by nanofiltration mass transfer mathematical model. Experiments showed the enhanced separation behavior, the decrease in the mass transfer coefficient while the increase in ethanol concentration from 20% to 40%, MWCO at 450 and pH 6.0. Under the same conditions, the enhanced separation behavior was appeared as the solvent changed into methanol and acetonitrile, the enhanced effect was positively correlated with the concentration of the three common organic solvents, and the effect order was acetonitrile>ethanol>methanol. This study took ephedrine as an example, and explored the mechanism of nanofiltration separation in the environment of organic solution, so as to provide references for nanofiltration separation for heat-sensitive traditional Chinese medicine of alkaloid.
Assuntos
Efedrina/química , Etanol , Metanol , Peso Molecular , SolventesRESUMO
The quality of traditional Chinese medicine affects the clinical efficacy and the market research at home or abroad, which is closely related to the standardization of production. At present, Chinese market still exist in drug quality and nonstandard production phenomenon. In addition to the existing GMP production standards, it is still necessary to ensure the authenticity and reliability of traditional Chinese medicine by means of retrospect. Based on the Xinshenghua granule, starting from the authenticity of the whole process of production, this study designs and constructs the traditional Chinese medicine traceability system which is equipped with the Internet platform by using two-dimensional code as a trace tool. By making authentic record of the production process and quality transfer, it is convenient for consumers to know the drug information. The production traceability system provides guarantee for the standardization of traditional Chinese medicine development, in order to obtain the production sourceï¼the testing quality, whereabouts and responsibility.
Assuntos
Medicamentos de Ervas Chinesas/normas , Medicina Tradicional Chinesa , Controle de Qualidade , Reprodutibilidade dos TestesRESUMO
Xinshenghua Keli is known as the "preferred prescription of postpartum", with large demand in the field of gynecologic medicine. However, the quality of the preparation is uneven in the market, so its clinical efficacy cannot be guaranteed. In order to improve and establish its quality control standard, high performance liquid chromatography (HPLC) was used to establish the fingerprint of Xinshenghua Keli. The detection was performed on Agilent 5 HC-C18 (2) column(4.6 mm×250 mm, 5 microns) with methanol-0.1% formic acid solution as mobile phase for gradient elution, at a flow rate of 1 mL·min⻹ with column temperature of 25 °C. The injection volume was 10 µL and detection wavelength was set at the maximum value between 210.0 nm and 400.0 nm by Photo-Diode Array (PDA) detector. The fingerprint of 12 batches of high-quality Xinshenghua Keli was established and 43 common peaks were identified. The similarities of crowned products, 10 batches of ordinary ones made by Jiangsu Rongyu Pharmaceutical and 10 batches produced by different manufacturers were evaluated. The composition identification and source analysis for the common peaks were performed by comparing the retention time of herbal medicines and ultraviolet absorption spectrum, along with high performance liquid chromatography-mass spectrometry (HPLC-MS) technology. The established fingerprint of Xinshenghua Keli, has proven to have good precision, stability and repeatability through the methodology validation, so it can be used to comprehensively evaluate the quality of Xinshenghua Keli.
Assuntos
Medicamentos de Ervas Chinesas/química , Compostos Fitoquímicos/análise , Plantas Medicinais/química , Cromatografia Líquida de Alta Pressão , Espectrometria de Massas , Controle de QualidadeRESUMO
Based on the solution-diffusion effect and the charge effect theory in nanofiltration separation, the correlation between initial concentration and mass transfer coefficient was constructed to establish a mathematic model of synephrine in mass transfer process and verify its applicability. The experimental results showed that there was a linear relationship between operation pressure and membrane flux. Meanwhile, the membrane flux was gradually decayed with the increase of solute concentration. Besides, mass transfer coefficient and initial concentration of synephrine showed power function correlation with each other by solution-diffusion effect and the charge effect, and the regression coefficients were greater than 0.9. The mass transfer coefficient of dissociation synephrine was less than that in the state of free and free-dissociation. Moreover, on the basis of power function relationship between mass transfer coefficient and initial concentration, the results showed that the predicted rejections of synephrine from Citrus aurantium water extract by use of the mathematical model approximated well to real ones, verifying that the model was practical and feasible. The unclear separation mechanism of nanofiltration for alkaloids was clarified preliminary by the predicted model of nanofiltration separation with synephrine as the example, providing theoretical and technical support for nanofiltration separation, especially for traditional Chinese medicine with alkaloids.
Assuntos
Citrus/química , Filtração , Sinefrina/química , Alcaloides/química , Modelos Teóricos , Extratos VegetaisRESUMO
To optimize the concentrate process of alkaloid from Leonurus japonicus by nanofiltration-ultrafiltration coupling technology with response surface methodology. The experiment showed that after ultrafiltration pre-treatment, the total protein removal rate was 94.38% in aqueous extract from L. japonicus, and the nanofiltration technology had obvious advantages over the conventional concentrate process. The optimal concentrate conditions were as followsï¼molecular weight cut-off 450, pH 3.07, concentration of stachydrine hydrochloride 80.15 mgâ¢L⻹, and concentration of the total alkaloid 285.73 mgâ¢L⻹. The cut-off rate was 93.37% and 95.85% respectively for stachydrine hydrochloride and the total alkaloid under the optimum conditions, with a relative error of 0.79% and 1.16% respectively. The combination of Box-Behnken design and response surface analysis can well optimize the concentrate process of L. japonicus by nanofiltration, and the results provide the basis for nanofiltration concentrate for heat-sensitive traditional Chinese medicine.
Assuntos
Alcaloides/isolamento & purificação , Leonurus/química , Ultrafiltração , Medicamentos de Ervas Chinesas , Medicina Tradicional ChinesaRESUMO
To separate chlorogenic acid from low concentration ethanol and explore the influence of Donnan effect and solution-diffusion effect on the nanofiltration separation rule. The experiment showed that solution pH and ethanol volume percent had influences on the separation of chlorogenic acid. Within the pH values from 3 to 7 for chlorogenic acid in 30% ethanol, the rejection rate of chlorogenic acid was changed by 70.27%. Through the response surface method for quadratic regression model, an interaction had been found in molecule weight cut-off, pH and ethanol volume percent. In fixed nanofiltration apparatus, the existence states of chlorogenic acid determinedits separation rules. With the increase of ethanol concentration, the free form chlorogenic acid was easily adsorbed, dissolved on membrane surface and then caused high transmittance due to the solution-diffusion effect. However, at the same time, due to the double effects of Donnan effect and solution-diffusion effect, the ionic state of chlorogenic acid was hard to be adsorbed in membrane surface and thus caused high rejection rate. The combination of Box-Behnken design and response surface analysis can well optimize the concentrate process by nanofiltration, and the results showed that nanofiltration had several big advantages over the traditional vacuum concentrate technology, meanwhile, and solved the problems of low efficiency and serious component lossesin the Chinese medicines separation process for low concentration organic solvent-water solution.
Assuntos
Ácido Clorogênico/isolamento & purificação , Etanol/isolamento & purificação , Filtração/métodos , Concentração de Íons de Hidrogênio , NanotecnologiaRESUMO
Two novel oleanane-type triterpene saponins, licorice-saponin P2 (1) and licorice-saponin Q2 (3), together with nine known compounds 2, 4-11, have been isolated from the water extract of the roots of Glycyrrhiza inflata. The structures of these compounds were elucidated on the basis of spectroscopic analysis, including 2D-NMR experiments (1H-1H COSY, HSQC, HMBC and ROESY). In in vitro assays, compounds 2-4, 6 and 11 showed significant hepatoprotective activities by lowering the ALT and AST levels in primary rat hepatocytes injured by D-galactosamine (D-GalN). In addition, compounds 2-4, 6, 7 and 11 were found to inhibit the activity of PLA2 with IC50 values of 6.9 µM, 3.6 µM, 16.9 µM, 27.1 µM, 32.2 µM and 9.3 µM, respectively, which might be involved in the regulation of the hepatoprotective activities observed.
Assuntos
Glycyrrhiza/química , Fígado/efeitos dos fármacos , Saponinas/farmacologia , Triterpenos/química , Animais , Galactosamina/toxicidade , Hepatócitos/efeitos dos fármacos , Extratos Vegetais/química , Raízes de Plantas/química , Cultura Primária de Células , Ratos , Saponinas/química , Triterpenos/farmacologiaRESUMO
Three new oleanane-type triterpene saponins, namely licorice-saponin M3 (1), licorice-saponin N4 (2), and licorice-saponin O4 (3), an artificial product (4), as well as five known triterpene glucuronides (5-9), were isolated from the roots of Glycyrrhiza glabra L. Their structures were established using 1D and 2D NMR spectroscopy, mass spectrometry, and by comparison with spectroscopic data reported in the literature. The inhibitory effects of the selected compounds on neuraminidase were evaluated, and the preliminary structure-activity relationship was also predicted.
Assuntos
Glycyrrhiza/química , Neuraminidase/antagonistas & inibidores , Ácido Oleanólico/análogos & derivados , Saponinas/isolamento & purificação , Antioxidantes , Estrutura Molecular , Ressonância Magnética Nuclear Biomolecular , Ácido Oleanólico/química , Ácido Oleanólico/isolamento & purificação , Ácido Oleanólico/farmacologia , Raízes de Plantas/química , Saponinas/química , Saponinas/farmacologia , Relação Estrutura-AtividadeRESUMO
Triterpenoid saponins, a major bioactive component of liquorice, possess high hydrophilicity and often co-occur with other impurities of similar polarity. Additionally, subtle structural differences of some triterpenoid saponins bring challenges to comprehensive characterisation. In this study, triterpenoid saponins of three Glycyrrhiza species were systematically analysed using rapid resolution liquid chromatography quadrupole time-of-flight mass spectrometry (RRLC-Q-TOF-MS) coupled with mass defect filtering (MDF). Firstly, comprehensive date acquisition was achieved using RRLC-Q-TOF-MS. Secondly, a polygonal MDF method was established by summarizing known and speculated substituents and modifications based on the core structure to rapidly screen potential triterpenoid saponins. Thirdly, based on the fragmentation patterns of reference compounds, an identification strategy for characterisation of triterpenoid saponins was proposed. The strategy divided triterpenoid saponins into three distinct classes. By this strategy, 98 triterpenoid saponins including 10 potential new ones were tentatively characterised. Finally, triterpenoid saponins of three Glycyrrhiza species were further analysed using principle component analysis (PCA) and orthogonality partial least squares discriminant analysis (OPLS-DA). Among these, 18 compounds with variable importance in projections (VIP) > 1.0 and P values < 0.05 were selected to distinguish three Glycyrrhiza species. Overall, our study provided a reference for quality control and rational use of the three species.