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1.
Small ; : e2310028, 2024 Apr 23.
Artículo en Inglés | MEDLINE | ID: mdl-38651514

RESUMEN

In this study, two novel donor-acceptor (D-A) copolymers are designed and synthesized, DTBT-2T and DTBT-2T2F with 2,2'-bithiophene or 3,3'-difluoro-2,2'-bithiophene as the donor unit and dithienobenzothiadiazole as the acceptor unit, and used them as donor materials in non-fullerene organic solar cells (OSCs). Due to enhanced planarity of polymer chains resulted by the intramolecular F···S noncovalent interactions, the incorporation of 3,3'-difluoro-2,2'-bithiophene unit instead of 2,2'-bithiophene into the polymers can enhance their molecular packing, crystallinity and hole mobility. The DTBT-2T:L8-BO based binary OSCs deliver a power conversion efficiency (PCE) of only 9.71% with a Voc of 0.78 V, a Jsc of 20.69 mA cm-2 , and an FF of 59.67%. Moreover, the introduction of fluoro atoms can lower the highest occupied molecular orbital levels. As a result, DTBT-2T2F:L8-BO based single-junction binary OSCs exhibited less recombination loss, more balanced charge mobility, and more favorable morphology, resulting in an impressive PCE of 17.03% with a higher Voc of 0.89 V, a Jsc of 25.40 mA cm-2, and an FF of 75.74%. These results indicate that 3,3'-difluoro-2,2'-bithiophene unit can be used as an effective building block to synthesize high performance polymer donor materials. This work greatly expands the selection range of donor units for constructing high-performance polymers.

2.
Molecules ; 29(9)2024 Apr 29.
Artículo en Inglés | MEDLINE | ID: mdl-38731534

RESUMEN

Two unreported heteropolysaccharides, denoted as YCJP-1 and YCJP-2, were isolated from the herbs of Chloranthus japonicus. YCJP-1 was a heteropolysaccharide composed of glucose, galactose, arabinose, mannose, rhamnose, and a minor proportion of uronic acids, with the molecular weight mainly distributed in the 74,475-228,443 Da range. YCJP-2 was mainly composed of glucose, mannose, and galactose, with the molecular weights ranging from 848 to 5810 Da. To further evaluate the anti-gastric cancer effects of C. japonicus, the inhibitory effects of the crude polysaccharide (YCJP) and the purified polysaccharides (YCJP-1 and YCJP-2) were determined using a CCK-8 assay and colon-forming assay on MGC-803 and AGS gastric cancer cell lines. Our results showed that YCJP, YCJP-1, and YCJP-2 possess prominent inhibitory effects on the proliferation of MGC-803 and AGS cells, and the AGS cell was more sensitive to YCJP, YCJP-1, and YCJP-2. Moreover, YCJP-2 demonstrated superior anti-gastric cancer effects compared to YCJP-1. This could potentially be attributed to YCJP-2's higher glucose content and narrower molecular weight distribution.


Asunto(s)
Proliferación Celular , Polisacáridos , Neoplasias Gástricas , Humanos , Polisacáridos/farmacología , Polisacáridos/química , Polisacáridos/aislamiento & purificación , Neoplasias Gástricas/tratamiento farmacológico , Neoplasias Gástricas/patología , Línea Celular Tumoral , Proliferación Celular/efectos de los fármacos , Extractos Vegetales/farmacología , Extractos Vegetales/química , Antineoplásicos Fitogénicos/farmacología , Antineoplásicos Fitogénicos/química , Antineoplásicos Fitogénicos/aislamiento & purificación , Peso Molecular , Caryophyllaceae/química
3.
Angew Chem Int Ed Engl ; : e202405949, 2024 Jun 13.
Artículo en Inglés | MEDLINE | ID: mdl-38871648

RESUMEN

Layer-by-layer (LbL) deposition of active layers in organic solar cells (OSCs) offers immense potential for optimizing performance through precise tailoring of each layer. However, achieving high-performance LbL OSCs with distinct solid additives in each layer remains challenging. In this study, we explore a novel approach that strategically incorporates different solid additives into specific layers of LbL devices. To this end, we introduce FeCl3 into the lower donor (D18) layer as a p-type dopant to enhance hole concentration and mobility. Concurrently, we incorporate the wide-bandgap conjugated polymer poly(9,9-di-n-octylfluorenyl-2,7-diyl) (PFO) into the upper acceptor (L8-BO) layer to improve the morphology and prolong exciton lifetime. Unlike previous studies, our approach combines these two strategies to achieve higher and more balanced electron and hole mobility without affecting device open-circuit voltage, while also suppressing charge recombination. Consequently, the power conversion efficiency (PCE) of the D18+FeCl3/L8-BO device increases to 18.12%, while the D18/L8-BO+PFO device attains a PCE of 18.79%. These values represent substantial improvements over the control device's PCE of 17.59%. Notably, when both FeCl3 and PFO are incorporated, the D18+FeCl3/L8-BO+PFO device achieves a remarkable PCE of 19.17%. In summary, our research results demonstrate the effectiveness of the layered solid additive strategy in improving OSC performance.

4.
Int Arch Allergy Immunol ; 184(11): 1099-1105, 2023.
Artículo en Inglés | MEDLINE | ID: mdl-37598674

RESUMEN

INTRODUCTION: Small airway dysfunction (SAD) is associated with type 2 inflammation in patients who have non-asthmatic chronic rhinosinusitis with nasal polyps (CRSwNPs); however, the risk factors for abnormal small airway function indicators in CRSwNP patients with and without asthma remain unclear. METHODS: We retrospectively analyzed 41 asthmatic and 109 non-asthmatic CRSwNP patients. Clinical characteristics were compared between groups, correlations between small airway function and clinical parameters were calculated, and independent risk factors for every small airway indicator were identified in each group. RESULTS: Asthmatic CRSwNP patients had significantly reduced small airway function, and the proportion of patients with SAD was higher in asthmatic CRSwNP patients (65.85%) than in patients without asthma (9.17%). With regard to specific airway function indicators, age and a patient's blood eosinophil (%) were identified as independent risk factors for lower FEF50% %pred and FEF25-75% pred, with age being an independent risk factor for FEF75% %pred in asthmatic CRSwNP patients. In non-asthmatic CRSwNP patients, allergic rhinitis comorbidity was found to be an independent risk factor for FEF50% %pred, FEF75% %pred, and FEF25-75% %pred. CONCLUSION: Physicians should pay greater attention to risk factors for abnormal small airway function indicators in patients with CRSwNPs to prevent the occurrence of SAD.


Asunto(s)
Asma , Pólipos Nasales , Rinitis , Sinusitis , Humanos , Pólipos Nasales/complicaciones , Pólipos Nasales/epidemiología , Estudios Retrospectivos , Rinitis/complicaciones , Rinitis/epidemiología , Asma/complicaciones , Asma/epidemiología , Sinusitis/complicaciones , Sinusitis/epidemiología , Factores de Riesgo , Enfermedad Crónica
5.
Molecules ; 28(6)2023 Mar 07.
Artículo en Inglés | MEDLINE | ID: mdl-36985397

RESUMEN

Recently, selenium nanoparticles have been drawing attention worldwide, and it is crucial to increase the stability of nano-Se. Morinda officinalis polysaccharides (MOP) are the main active component in Morinda officinalis radix. However, their low activity has limited their application. A novel selenium nanoparticle (Se-MOP) was prepared to solve these problems using MOP as a dispersant. The zeta potential was measured to evaluate the stability, and UV and ATR-FTIR were used to investigate the binding type of selenium and MOP. The morphology was observed by the TEM method. Furthermore, the inhibitory effect on five selected cancer cells (HepG2, MCF-7, AGS, PC9, and HCT8) was evaluated, showing remarkable inhibition of all five cancer cells. The mechanism of inhibition was also investigated by cell circle assay, and it was found that Se-MOP could induce cell circle G0/G1 phase arrest. Immune-enhancing activities were evaluated by measuring the proliferation and cytokines of mouse spleen lymphocytes in vitro and quantitative RT-PCR. The results indicated that single stimulation of Se-MOP and synergistic stimulation with PHA or LPS increased immune capacity and improved immune by increasing the expression of cytokines.


Asunto(s)
Morinda , Nanopartículas , Selenio , Ratones , Animales , Selenio/farmacología , Selenio/química , Morinda/química , Polisacáridos/farmacología , Citocinas , Nanopartículas/química
6.
Angew Chem Int Ed Engl ; 62(50): e202314420, 2023 Dec 11.
Artículo en Inglés | MEDLINE | ID: mdl-37881111

RESUMEN

In this work, inspired by the principles of a pressure cooker, we utilized a high-pressure method to address the processing challenges associated with high molecular weight polymers. Through this approach, we successfully dissolved high molecular weight D18 in chloroform at 100 °C within a pressure-tight vial. The increased steam pressure raised the boiling point and dissolving capacity of chloroform, enabling the creation of a hybrid film with superior properties, including more ordered molecular arrangement, increased crystallinity, extended exciton diffusion length, and improved phase morphology. Organic solar cells (OSCs) based on D18 : L8-BO prepared using this high-pressure method achieved an outstanding power conversion efficiency of 19.65 %, setting a new record for binary devices to date. Furthermore, this high-pressure method was successfully applied to fabricate OSCs based on other common systems, leading to significant enhancements in device performance. In summary, this research introduces a universal method for processing high molecular weight D18 materials, ultimately resulting in the highest performance reported for binary organic solar cells.

7.
Small ; 18(35): e2203454, 2022 Sep.
Artículo en Inglés | MEDLINE | ID: mdl-35934890

RESUMEN

Motivated by simplifying the synthesis of nonfullerene acceptor and establishing the relation between molecular structure and photovoltaic performance, two isomeric nonfused ring electron acceptors (o-TT-Cl and m-TT-Cl), whose properties can be adjusted by changing the side chains, are designed and synthesized with several high-yield steps. o-TT-Cl with V-shaped side chain induces a dominated J-aggregation and displays much better solubility and more ordered packing than m-TT-Cl with linear side chain. Thus, the o-TT-Cl-based blend film generates better phase morphology and charge transport than m-TT-Cl-based one. Finally, the power conversion efficiency of o-TT-Cl-based devices is 12.84%, which is much higher than that of m-TT-Cl-based ones (6.54%). This work highlights the importance of side chains engineering on improving photovoltaic performance of nonfused ring electron acceptors.

8.
Molecules ; 26(6)2021 Mar 19.
Artículo en Inglés | MEDLINE | ID: mdl-33808811

RESUMEN

Deep eutectic solvents (DESs) are considered as efficient and green solvents for the extraction of bioactive compounds from medicinal plants. In this work, a novel method of DES-based ultrasound-assisted extraction of bioactive compounds from Baphicacanthus cusia leaves (BCL) was established. Systematic screening and the morphology of the original and treated BCL were observed with scanning electron microscopy to determine the extraction efficiency of different solvents. The extraction conditions were optimized by Box-Behnken design (BBD) tests and the optimal extraction conditions were as follows: lactic acid/L-menthol ratio of 5: 2 (mol/mol), solid-liquid ratio of 80.0 mL/g and temperature of 60.5 °C. The extraction yields of tryptanthrin, indigo and indirubin reached 0.356, 1.744 and 0.562 mg/g, respectively. The results of a 2,2-diphenyl-1-picrylhydrazy (DPPH) radical scavenging activity test indicated the feasibility of DESs in the extraction of bioactive compounds. This study indicated that L-menthol/lactic acid was a green and efficient solvent for the extraction of bioactive compounds from BCL, and DES-based ultrasound-assisted extraction could be used as an effective application strategy for the extraction of bioactive compounds from medicinal plants.


Asunto(s)
Acanthaceae/química , Fitoquímicos/aislamiento & purificación , Extractos Vegetales/química , Hojas de la Planta/química , Tecnología Química Verde , Calor , Fitoquímicos/química , Solventes/química
9.
Molecules ; 26(23)2021 Nov 29.
Artículo en Inglés | MEDLINE | ID: mdl-34885827

RESUMEN

A method based on high performance liquid chromatography with evaporative light scattering detection (HPLC-ELSD) was developed for the quantitative analysis of three active compounds and chemical fingerprint analyses of saccharides in Morindae officinalis radix. Ten batches of Morindae officinalis radix were collected from different plantations in the Guangdong region of China and used to establish the fingerprint. The samples were separated with a COSMOIL Sugar-D column (4.6 mm × 250 mm, 5 µm) by using gradient elution with water (A) and acetonitrile (B). In addition, Trapped-Ion-Mobility (tims) Time-Of-Flight (tims TOF) was used to identify saccharides of Morindae officinalis radix. Fingerprint chromatogram presented 26 common characteristic peaks in the roots of Morinda officinalis How, and the similarities were more than 0.926. In quantitative analysis, the three compounds showed good regression (r = 0.9995-0.9998) within the test ranges, and the recoveries of the method were in the range of 96.7-101.7%. The contents of sucrose, kestose and nystose in all samples were determined as 1.21-7.92%, 1.02-3.37%, and 2.38-6.55%, respectively. The developed HPLC fingerprint method is reliable and was validated for the quality control and identification of Morindae officinalis radix and can be successfully used to assess the quality of Morindae officinalis radix.


Asunto(s)
Medicamentos Herbarios Chinos , Oligosacáridos , Dispersión de Radiación , Cromatografía Líquida de Alta Presión , Medicamentos Herbarios Chinos/química , Modelos Lineales , Oligosacáridos/análisis , Oligosacáridos/aislamiento & purificación , Análisis de Componente Principal , Reproducibilidad de los Resultados
10.
Molecules ; 26(9)2021 May 02.
Artículo en Inglés | MEDLINE | ID: mdl-34063301

RESUMEN

Amomum Villosum Lour. (A. villosum) is a folk medicine that has been used for more than 1300 years. However, study of the polysaccharides of A. villosum is seriously neglected. The objectives of this study are to explore the structural characteristics of polysaccharides from A. villosum (AVPs) and their effects on immune cells. In this study, the acidic polysaccharides (AVPG-1 and AVPG-2) were isolated from AVPs and purified via anion exchange and gel filtration chromatography. The structural characteristics of the polysaccharides were characterized by methylation, HPSEC-MALLS-RID, HPLC, FT-IR, SEM, GC-MS and NMR techniques. AVPG-1 with a molecular weight of 514 kDa had the backbone of → 4)-α-d-Glcp-(1 → 3,4)-ß-d-Glcp-(1 → 4)-α-d-Glcp-(1 →. AVPG-2 with a higher molecular weight (14800 kDa) comprised a backbone of → 4)-α-d-Glcp-(1 → 3,6)-ß-d-Galp-(1 → 4)-α-d-Glcp-(1 →. RAW 264.7 cells were used to investigate the potential effect of AVPG-1 and AVPG-2 on macrophages, and lipopolysaccharide (LPS) was used as a positive control. The results from bioassays showed that AVPG-2 exhibited stronger immunomodulatory activity than AVPG-1. AVPG-2 significantly induced nitric oxide (NO) production as well as the release of interleukin (IL)-6 and tumor necrosis factor alpha (TNF-α), and upregulated phagocytic capacities of RAW 264.7 cells. Real-time PCR analysis revealed that AVPG-2 was able to turn the polarization of macrophages to the M1 direction. These results suggested that AVPs could be explored as potential immunomodulatory agents of the functional foods or complementary medicine.


Asunto(s)
Amomum/química , Polisacáridos/química , Polisacáridos/metabolismo , Animales , Supervivencia Celular , Cromatografía Líquida de Alta Presión , Citocinas/metabolismo , Etanol , Factores Inmunológicos , Inmunomodulación/efectos de los fármacos , Lipopolisacáridos/química , Macrófagos/metabolismo , Espectroscopía de Resonancia Magnética , Ratones , Microscopía Electrónica de Rastreo , Peso Molecular , Óxido Nítrico/química , Fagocitosis , Células RAW 264.7 , Espectroscopía Infrarroja por Transformada de Fourier , Propiedades de Superficie
11.
Prep Biochem Biotechnol ; 49(4): 360-367, 2019.
Artículo en Inglés | MEDLINE | ID: mdl-30822196

RESUMEN

Hepatic stimulator substance (HSS) is prepared by the freeze-thaw method on a large scale, but it is time-consuming and inefficient. It is necessary to find a better method to improve the efficiency and yield of HSS. In this study, HSS was prepared by enzymatic hydrolysis of neonatal porcine liver with trypsin, papain, dispase, and alcalase. Relatively, dispase was found to be the best enzyme, based on the results of the degree of hydrolysis and MTT assay. Box-Behnken design-response surface method was used to optimize the conditions, which were as follows: enzyme (dispase) concentration, 4164 U/g; substrate concentration, 7% (w/v); hydrolysis time, 4.3 hr; temperature, 45 °C; and pH, 6.5. The degree of hydrolysis was (54.99 ± 1.57)%. Shotgun proteomics coupled with Gene Ontology (GO) analysis based on the PANTHER classification system was used to screen proteins from neonatal porcine liver. The results profiled the proteins into biological processes, molecular functions, and cellular components, thus laying a foundation for further studies on components involved in and mechanisms of liver regeneration. Overall, the results suggest that enzymatic hydrolysis might be a promising method for industrial application.


Asunto(s)
Hígado/química , Péptidos/química , Proteínas/química , Animales , Cromatografía Liquida/métodos , Endopeptidasas/química , Hidrólisis , Péptidos/análisis , Péptidos/aislamiento & purificación , Proteínas/análisis , Proteínas/aislamiento & purificación , Proteómica/métodos , Porcinos , Espectrometría de Masas en Tándem/métodos
12.
J Sep Sci ; 41(9): 2092-2101, 2018 May.
Artículo en Inglés | MEDLINE | ID: mdl-29385309

RESUMEN

The objective of this study was to develop a consecutive preparation method for the isolation and purification of hainanmurpanin, meranzin, and phebalosin from leaves of Murraya exotica L. The process involved supercritical fluid extraction with CO2 , solvent extraction, and two-step high-speed countercurrent chromatography. Pressure, temperature, and the volume of entrainer were optimized as 27 MPa, 52°C, and 60 mL by response surface methodology in supercritical fluid extraction with CO2 , and the yield of the crude extracts was 7.91 g from 100 g of leaves. Subsequently, 80% methanol/water was used to extract and condense the three compounds from the crude extracts, and 4.23 g of methanol/water extracts was obtained. Then, a two-step high-speed countercurrent chromatography procedure was developed for the isolation of the three target compounds from methanol/water extracts, including conventional high-speed countercurrent chromatography for further enrichment and consecutive high-speed countercurrent chromatography for purification. The yield of concentrates from high-speed countercurrent chromatography was 2.50 g from 4.23 g of methanol/water extracts. Finally, the consecutive high-speed countercurrent chromatography produced 103.2 mg of hainanmurpanin, 244.7 mg of meranzin, and 255.4 mg of phebalosin with purities up to 97.66, 99.36, and 98.64%, respectively, from 900 mg of high-speed countercurrent chromatography concentrates in one run of three consecutive sample loadings without exchanging a solvent system.


Asunto(s)
Cumarinas/aislamiento & purificación , Murraya/química , Hojas de la Planta/química , Cromatografía Líquida de Alta Presión , Cromatografía con Fluido Supercrítico , Distribución en Contracorriente , Extractos Vegetales/química , Presión , Solventes , Temperatura
13.
J Sci Food Agric ; 98(7): 2498-2506, 2018 May.
Artículo en Inglés | MEDLINE | ID: mdl-29023749

RESUMEN

BACKGROUND: Supercritical fluid extraction with CO2 (SFE-CO2 ) was utilized for extraction of capsaicin (CA) and dihydrocapsaicin (DHCA) from Capsici Fructus, and then a two-step enrichment method for separating capsaicinoids from SFE-CO2 extracts was developed. The process involved extraction with aqueous methanol and crystallization by alkali extraction and acid precipitation. Finally, a consecutive high-speed countercurrent chromatography (HSCCC) separation method was successfully applied in the purification of CA and DHCA from capsaicinoid crystal. RESULTS: The extraction pressure, extraction temperature and volume of co-solvent were optimized at 33 MPa, 41 °C and 75 mL, respectively, using response surface methodology; the extraction rates of CA and DHCA were about 93.18% and 93.49%, respectively. 407.43 mg capsaicinoid crystal was isolated from the SFE-CO2 extracts obtained from 100 g capsicum powder by the two-step enrichment method. About 506 mg and 184 mg CA and DHCA with purities up to 98.31% and 96.68%, respectively, were obtained from 1 g capsaicinoid crystal in one HSCCC of three consecutive sample loadings without exchanging any solvent system. CONCLUSIONS: This method comprising SFE-CO2 , a two-step enrichment and HSCCC was efficient, powerful and practical for the large-scale preparation of CA and DHCA from Capsici Fructus with high purity and high yield. © 2017 Society of Chemical Industry.


Asunto(s)
Capsaicina/análogos & derivados , Capsaicina/aislamiento & purificación , Capsicum/química , Cromatografía con Fluido Supercrítico/métodos , Distribución en Contracorriente/métodos , Extractos Vegetales/aislamiento & purificación , Capsaicina/química , Frutas/química , Extractos Vegetales/química
14.
J Am Chem Soc ; 139(9): 3356-3359, 2017 03 08.
Artículo en Inglés | MEDLINE | ID: mdl-28225257

RESUMEN

We have developed a kind of novel fused-ring small molecular acceptor, whose planar conformation can be locked by intramolecular noncovalent interaction. The formation of planar supramolecular fused-ring structure by conformation locking can effectively broaden its absorption spectrum, enhance the electron mobility, and reduce the nonradiative energy loss. Polymer solar cells (PSCs) based on this acceptor afforded a power conversion efficiency (PCE) of 9.6%. In contrast, PSCs based on similar acceptor, which cannot form a flat conformation, only gave a PCE of 2.3%. Such design strategy, which can make the synthesis of small molecular acceptor much easier, will be promising in developing a new acceptor for high efficiency polymer solar cells.

15.
J Sep Sci ; 40(6): 1273-1282, 2017 Mar.
Artículo en Inglés | MEDLINE | ID: mdl-28106330

RESUMEN

10-Deacetylbaccatin III, an important semisynthetic precursor of paclitaxel and docetaxel, can be extracted from Taxus wallichiana Zucc. A process for the isolation and purification of 10-deacetylbaccatin III (1), baccatin III (2), and 7ß-xylosyl-10-deacetyltaxol (3) from the leaves and branches of Taxus wallichiana Zucc. via macroporous resin column chromatography combined with high-speed countercurrent chromatography or reversed-phase flash chromatography was developed in this study. After fractionation by macroporous resin column chromatography, 80% methanol fraction was selected based on high-performance liquid chromatography and liquid chromatography with mass spectrometry qualitative analysis. A solvent system composed of n-hexane, ethyl acetate, methanol, and water (1.6:2.5:1.6:2.5, v/v/v/v) was used for the high-speed countercurrent chromatography separation at a flow rate of 2.5 mL/min. The reversed-phase flash chromatography separation was performed using methanol/water as the mobile phase at a flow rate of 3 mL/min. The high-speed countercurrent chromatography separation produced compounds 1 (10.2 mg, 94.4%), 2 (2.1 mg, 98.0%), and 3 (4.6 mg, 98.8%) from 100 mg of sample within 110 min, while the reversed-phase flash chromatography separation purified compounds 1 (9.8 mg, 95.6%) and 3 (4.9 mg, 97.9%) from 100 mg of sample within 120 min.


Asunto(s)
Hidrocarburos Aromáticos con Puentes/aislamiento & purificación , Extractos Vegetales/química , Taxoides/aislamiento & purificación , Taxus/química , Cromatografía Líquida de Alta Presión , Distribución en Contracorriente
16.
Biomed Chromatogr ; 29(4): 626-32, 2015 Apr.
Artículo en Inglés | MEDLINE | ID: mdl-25251881

RESUMEN

In this study, a novel solidification of floating organic drop liquid-phase microextraction cell fishing with gas chromatography-mass spectrometry (SFOD-LPME-CF-GC-MS) method was established and used to screen, isolate and analyze bioactive components from Amomum villosum Lour. extract. Through comparision of its effect on the models of normal cell and inflammatory cells, anti-inflammatory active components of essential oil from A. villosum Lour. were readily screened, and the components obtained are in agreement with related pharmacological articles. SFOD-LPME-CF-GC-MS was used to analyze the interaction of A. villosum Lour. extracts with normal and lipopolysaccharide-stimulated RAW264.7 macrophage cells. The effect of A. villosum Lour. essential oil extracts in the LPS-stimulated RAW264.7 model were also assessed in terms of cytotoxicity and nitric oxide production as an indication of bioactivity. Three potentially bioactive components were identified, demonstrating that SFOD-LPME-CF-GC-MS can be used successfully in the drug-screening process. This approach avoids the requirement for protein precipitation, but more importantly, generates a high concentration ratio, allowing analysis of trace components in traditional Chinese medicines. SFOD-LPME-CF-GC-MS is a simple, fast, effective and reliable method for the screening and analysis of bioactive components, and it can be extended to screen other bioactive components from TCMs.


Asunto(s)
Amomum/química , Medicamentos Herbarios Chinos/química , Medicamentos Herbarios Chinos/aislamiento & purificación , Cromatografía de Gases y Espectrometría de Masas/métodos , Microextracción en Fase Líquida/métodos , Animales , Antiinflamatorios/química , Antiinflamatorios/aislamiento & purificación , Antiinflamatorios/farmacología , Línea Celular , Medicamentos Herbarios Chinos/farmacología , Macrófagos/efectos de los fármacos , Macrófagos/inmunología , Ratones , Aceites Volátiles/química , Aceites Volátiles/aislamiento & purificación , Aceites Volátiles/farmacología
17.
J Sep Sci ; 37(17): 2322-30, 2014 Sep.
Artículo en Inglés | MEDLINE | ID: mdl-24945899

RESUMEN

A consecutive preparation method for the isolation and purification of paclitaxel from the Taxus Chinensis cell culture was developed in this study. The process involved alkaline Al2O3 chromatography, fractional precipitation, and high-speed countercurrent chromatography. The original cell culture materials were first extracted with methanol using ultrasound-assisted extraction, and then the extract (the content of paclitaxel is 1.5%) was separated by alkaline Al2O3 column chromatography. Subsequently, fractional precipitation was used to obtain paclitaxel. In particular, response surface methodology was used to optimize the factors of fractional precipitation (methanol concentration, material-to-solvent ratio, and precipitating time were optimized as 48.14%, 8.85 mg/mL, and 48.71 h, respectively) and the yield of fractional precipitation product was 30.64 ± 0.60 mg (the content of paclitaxel is 89.3%, 27.37 ± 0.54 mg) from a 100 mg fraction by Al2O3 column separation (the content of paclitaxel is 32.4%). Then, the product was used for further isolation by high-speed countercurrent chromatography. About 1.00 g paclitaxel (200 ± 2 mg in each loading) with a purity up to 99.61% was isolated from 1.25 g of fractional precipitation product with a solvent system of n-hexane/ethyl acetate/methanol/water (1.2:1.8:1.5:1.5, v/v/v/v) in one run of five consecutive sample loadings without exchanging a new solvent system.


Asunto(s)
Distribución en Contracorriente/métodos , Medicamentos Herbarios Chinos/aislamiento & purificación , Precipitación Fraccionada/métodos , Paclitaxel/aislamiento & purificación , Taxus/química , Técnicas de Cultivo de Célula , Medicamentos Herbarios Chinos/química , Paclitaxel/química , Taxus/crecimiento & desarrollo
18.
J Sep Sci ; 37(8): 957-65, 2014 Apr.
Artículo en Inglés | MEDLINE | ID: mdl-24515421

RESUMEN

A method of ultrasonic-assisted extraction followed by high-speed countercurrent chromatography was established for the extraction and isolation of three flavonoid glycosides, i.e. rutin, narcissin, and nicotiflorin from Flos Sophorae Immaturus. The effects of ultrasonic-assisted extraction factors for the main flavonoid compound (rutin) from Flos Sophorae Immaturus were optimized using Box-Behnken design combined with response surface methodology. The optimum conditions were determined as ultrasonic power 83% (600 W), solvent-to-material ratio 56:1, methanol concentration 82% v/v, and extraction time 60 min. Three bioactive flavonol glucosides, rutin, narcissin, and nicotiflorin were isolated from Flos Sophorae Immaturus using high-speed countercurrent chromatography. The separation was performed with a two-phase solvent system containing ethyl acetate/n-butanol/methanol/water (4:0.9:0.2:5, v/v). Amounts of 87 mg of rutin, 10.8 mg of narcissin, and 1.8 mg of nicotiflorin were isolated from 302 mg of crude extract of Flos Sophorae Immaturus in a one-step separation within 160 min with purities of 99.3, 98.0, and 95.1%, respectively, as determined by HPLC with diode array detection. Their structures were characterized by UV, MS, and NMR spectroscopy. It was demonstrated that the established method was simple, fast, and convenient, which was feasible to extract and isolate active flavonoid glycosides from Flos Sophorae Immaturus.


Asunto(s)
Acústica , Fabaceae/química , Flavonoides/aislamiento & purificación , Flavonoles/aislamiento & purificación , Flores/química , Fenoles/aislamiento & purificación , Rutina/aislamiento & purificación , Distribución en Contracorriente , Flavonoides/química , Flavonoles/química , Fenoles/química , Rutina/química
19.
Phytochem Anal ; 25(3): 266-72, 2014.
Artículo en Inglés | MEDLINE | ID: mdl-24497376

RESUMEN

INTRODUCTION: Poplar tree gum has a similar chemical composition and appearance to Chinese propolis (bee glue) and has been widely used as a counterfeit propolis because Chinese propolis is typically the poplar-type propolis, the chemical composition of which is determined mainly by the resin of poplar trees. The discrimination of Chinese propolis from poplar tree gum is a challenging task. OBJECTIVE: To develop a rapid thin-layer chromatographic (TLC) identification method using chemometric fingerprinting to discriminate Chinese propolis from poplar tree gum. METHODS: A new TLC method using a combination of ammonia and hydrogen peroxide vapours as the visualisation reagent was developed to characterise the chemical profile of Chinese propolis. Three separate people performed TLC on eight Chinese propolis samples and three poplar tree gum samples of varying origins. Five chemometric methods, including similarity analysis, hierarchical clustering, k-means clustering, neural network and support vector machine, were compared for use in classifying the samples based on their densitograms obtained from the TLC chromatograms via image analysis. RESULTS: Hierarchical clustering, neural network and support vector machine analyses achieved a correct classification rate of 100% in classifying the samples. A strategy for TLC identification of Chinese propolis using chemometric fingerprinting was proposed and it provided accurate sample classification. CONCLUSION: The study has shown that the TLC identification method using chemometric fingerprinting is a rapid, low-cost method for the discrimination of Chinese propolis from poplar tree gum and may be used for the quality control of Chinese propolis.


Asunto(s)
Cromatografía en Capa Delgada/métodos , Populus/química , Própolis/aislamiento & purificación , Resinas de Plantas/aislamiento & purificación , Animales , Abejas , Análisis por Conglomerados , Mapeo Peptídico , Própolis/química , Resinas de Plantas/química , Árboles
20.
Eur J Drug Metab Pharmacokinet ; 39(1): 17-24, 2014 Mar.
Artículo en Inglés | MEDLINE | ID: mdl-23673491

RESUMEN

The purpose of this study was to investigate the effect of natural borneol (NB) on the pharmacokinetics and distribution of nimodipine in mice. A single dose of nimodipine was administered intravenously (2 mg/kg) to mice pretreated with NB (250 mg/kg) or vehicle. Blood as well as brain, liver, and kidney tissue samples were collected at 5, 10, 20, 40, and 60 min post-dose nimodipine. The concentrations of nimodipine in plasma and tissues were determined by ultra performance liquid chromatography (UPLC) coupled with UV detection, and the pharmacokinetic parameters were calculated based on non-compartmental analysis. NB increased the plasma AUC5-60 min by 26 % compared to the vehicle. In addition, brain concentrations of nimodipine in NB-treated mice were significantly higher than those in control mice with the increased AUC5-60 min by 30 %. In liver and kidney, NB also caused 26 and 47 % increase in AUC5-60 min, respectively. These results implicated that NB may inhibit the metabolism or elimination of nimodipine and enhance its distribution in brain and kidney tissue.


Asunto(s)
Bloqueadores de los Canales de Calcio/farmacocinética , Canfanos/administración & dosificación , Nimodipina/farmacocinética , Animales , Área Bajo la Curva , Biotransformación , Encéfalo/efectos de los fármacos , Encéfalo/metabolismo , Bloqueadores de los Canales de Calcio/administración & dosificación , Bloqueadores de los Canales de Calcio/sangre , Cromatografía Líquida de Alta Presión , Interacciones Farmacológicas , Inyecciones Intravenosas , Riñón/efectos de los fármacos , Riñón/metabolismo , Hígado/efectos de los fármacos , Hígado/metabolismo , Masculino , Ratones , Nimodipina/administración & dosificación , Nimodipina/sangre , Espectrofotometría Ultravioleta , Distribución Tisular
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