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1.
Biomed Chromatogr ; 33(12): e4692, 2019 Dec.
Artigo em Inglês | MEDLINE | ID: mdl-31452210

RESUMO

Ginkgo diterpene lactone (GDL) is the raw material for ginkgo diterpene lactone meglumine injection, which is used for treating cerebral ischemia. The aims of this study were to explore the cellular pharmacokinetics of GDL in whole cells and subcellular fractions, and detect cellular pharmacodynamics on the human SH-SY5Y cells induced by oxygen-glucose deprivation and reoxygenation (OGD/R). Firstly, a simple, sensitive and reliable liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for assessing the amount of ginkgolide A (GA), B (GB) and K (GK) in cellular/subcellular samples. Then, phosphatidylserine and mitochondria membrane potential were assayed to evaluate the extent of apoptosis effect. The study showed that the cellular/subcellular accumulation of GA and GB were increased in a concentration-dependent manner; the levels of GA and GB in cytosol were the highest among these subcellular organelles. Meanwhile, GDL also attenuated the OGD/R-induced increases in the percentage of apoptotic and mitochondria membrane potential. In addition, verapamil increased the rate and amount of GA and GB entering cellular/subcellular compartments through inhibition of P-glycoprotein activity, and promoted the protective effect of GDL. The present study reports the cellular pharmacokinetics profiles of GA and GB in normal and OGD/R-induced SH-SY5Y cells in vitro for the first time, which provided valuable information for clinical safety application.


Assuntos
Membro 1 da Subfamília B de Cassetes de Ligação de ATP , Diterpenos , Ginkgo biloba/química , Lactonas , Membro 1 da Subfamília B de Cassetes de Ligação de ATP/antagonistas & inibidores , Membro 1 da Subfamília B de Cassetes de Ligação de ATP/metabolismo , Linhagem Celular Tumoral , Sobrevivência Celular/efeitos dos fármacos , Cromatografia Líquida , Diterpenos/química , Diterpenos/farmacocinética , Diterpenos/farmacologia , Humanos , Lactonas/química , Lactonas/farmacocinética , Lactonas/farmacologia , Limite de Detecção , Modelos Lineares , Potencial da Membrana Mitocondrial/efeitos dos fármacos , Extratos Vegetais/química , Reprodutibilidade dos Testes , Espectrometria de Massas em Tandem
2.
Zhongguo Zhong Yao Za Zhi ; 44(2): 298-307, 2019 Jan.
Artigo em Zh | MEDLINE | ID: mdl-30989949

RESUMO

The study aims to qualitatively analyze the chemical composition of compound Nanxing acesodyne plaster by ultra-high performance liquid chromatography-quadrupole time-of-flight mass spectrometry( UPLC-Q-TOF-MS/MS). The analysis was performed on Agilent Zorbax SB-C_(18)( 4. 6 mm×250 mm,5 µm) column. The mobile phase consisted of methanol and 0. 2% formic acid-water was used as gradient elution. The flow rate was 1 mL·min~(-1) and column temperature was 30 ℃. The Mass spectrometry was acquired in both positive and negative ion modes using ESI. The components were identified by the precise mass-to-charge ratio,secondary fragmentation and other information combined with reference substance and literature data. As a result,58 compounds were identified and predicted,including alkaloids,flavonoids,coumarins,organic acids and lactone compounds,of which 12 compounds were verified by the reference substances. The results provide reference for the quality control of compound Nanxing acesodyne plaster,and lay the foundation for elucidating the active components mechanism.


Assuntos
Cromatografia Líquida de Alta Pressão , Medicamentos de Ervas Chinesas/química , Compostos Fitoquímicos/análise , Espectrometria de Massas em Tandem
3.
Zhongguo Zhong Yao Za Zhi ; 44(13): 2675-2679, 2019 Jul.
Artigo em Zh | MEDLINE | ID: mdl-31359676

RESUMO

As an important integral part of traditional Chinese medicine chemical biology( TCMCB),it is of great importance to rapid isolate,and reliably identify the chemical components in herbal medicines. Phytochemical studies on the anti-inflammatory active part of Chinese dragon's blood,the red resin of Dracaena cochinchinensis,resulted in the isolation of two compounds,nordracophane( 1) and dracophane( 2),using LC-MS and chromatographic techniques( Silica gel,ODS and preparative HPLC). The structures,cyclic dihydrochalcane trimers,were elucidated on the basis of 1 D and 2 D NMR,MS,IR and UV spectral analysis. Compound 1 is a new compound,and 2 is isolated from D. cochinchinensis for the first time. Both compounds exhibited significant inhibition of nitric oxide production in lipopolysaccharides( LPS)-stimulated RAW264. 7 cells with IC50 values of( 14. 9±4. 50) and( 9. 0±0. 7) µmol·L-1.


Assuntos
Anti-Inflamatórios/isolamento & purificação , Espectrometria de Massas , Extratos Vegetais/isolamento & purificação , Animais , Cromatografia Líquida , Dracaena , Camundongos , Óxido Nítrico/metabolismo , Células RAW 264.7
4.
Zhongguo Zhong Yao Za Zhi ; 44(1): 150-157, 2019 Jan.
Artigo em Zh | MEDLINE | ID: mdl-30868826

RESUMO

Ten fractions(A-J) were prepared by separation of Longxue Tongluo Capsules(LTC) by using silica gel column chromatography and orthogonal experimental design,showing similar chemical profiles with different abundances of peaks.These ten samples were assessed with UHPLC-QE OrbitrapHRMS for 97 common peaks.For the pharmacological activity experiment,three kinds of in vitro cell models including lipopolysaccharide(LPS)-induced BV-2 microglial cells NO release model,oxygen-glucose deprivation/reoxygenation(OGD/R)-treated HUVEC vascular endothelial cells injury model,and OGD/R-treated PC-12 nerve cells injury model were employed to evaluated the bioactivity of each fraction.Based on the contribution of each identified component,grey relation analysis and partial least squares(PLS) analysis were performed to establish component-activity relationship of LTC,identify the potential active components.After that,validation of the potential active components in LTC was carried out by using the same models.The results indicated that 4 phenolic compounds including 7,4'-dihydroxyhomoisoflavanone,loureirin C,4,4'-dihydroxy-2,6-dimethoxydihydrochalcone,and homoisosocotrin-4'-ol,might be the active components for anti-neuroinflammation effect;five phenolic compounds such as 3,5,7,4'-tetrahydroxyhomoisoflavanone,loureirin D,7,4'-dihydroxyhomoisoflavane,and 5,7-dihydroxy-4'-methoxy-8-methyflavane,might have positive effects on the vascular endothelial injury;three phenolic compounds including 5,7,4'-trihydroxyflavanone,7,4'-dihydroxy-5-methoxyhomoisoflavane,and loureirin D,might be the active components in LTC against neuronal injury.


Assuntos
Isquemia Encefálica/tratamento farmacológico , Medicamentos de Ervas Chinesas/farmacologia , Células Endoteliais da Veia Umbilical Humana/efeitos dos fármacos , Microglia/efeitos dos fármacos , Cápsulas , Linhagem Celular , Glucose , Humanos , Oxigênio
5.
Zhongguo Zhong Yao Za Zhi ; 43(21): 4240-4247, 2018 Nov.
Artigo em Zh | MEDLINE | ID: mdl-30583624

RESUMO

The qualitative analysis method of RRLC-Q-TOF-MS/MS was established for determine the chemical constituents in Qige Keli. Kramosil C18 column (4.6 mm×150 mm, 3.5 µm) was used at the temperature of 30 °C. The mobile phase was 0.2% formic acid and acetonitrile by gradient elution, with a flow rate at 1.0 mL·min⁻¹, and the injection volume was 10 µL. The high-resolution quadrupole time-flight mass spectrometry was used as detector with electrospray ion source in both positive and negative models. On the basis of medicinal materials, reference materials, literature reports, and mass spectrometry data, the chemical composition in the Qige Keli was identified. A total of 44 compounds were identified, including 3 flavonoids, 21 flavonoid glycosides, 8 organic acids, 6 lactones, and 3 saponins. The results laid the foundation for the quality control of Qige Keli and the further research on pharmacodynamic materials.


Assuntos
Medicamentos de Ervas Chinesas/química , Compostos Fitoquímicos/análise , Ácidos/análise , Flavonoides/análise , Glicosídeos/análise , Lactonas/análise , Saponinas/análise , Espectrometria de Massas por Ionização por Electrospray , Espectrometria de Massas em Tandem
6.
Zhongguo Zhong Yao Za Zhi ; 43(7): 1392-1403, 2018 Apr.
Artigo em Zh | MEDLINE | ID: mdl-29728028

RESUMO

Platelet activating factor(PAF), an endogenous synthesized phospholipid transmitter, has widely biological activities. It has "signal transmission" effect in various life processes, but abnormality of concentration in vivo will promote or aggravate the diseases, such as, cerebral ischemia, myocardial injury, multi-organ failure, asthma, injury of liver and kidney, severely affecting the normal life activities of body. In recent years, with the development of medical science and technology, more and more attention has been paid to the research of platelet activating factor receptor antagonist. Components of animals, plants, microbial fermentation, and synthetic composition all can reflect such activity. Ginkgolide B and cytopone are the most representative herbal compositions at present. This paper referred to the research status of platelet activating factor receptor antagonist in recent years, made a summary of the researches on biological effect of platelet activating factor and platelet receptor antagonist of different sources, so as to provide a reference for the exploration of effective and safe platelet activating factor receptor antagonists.


Assuntos
Fator de Ativação de Plaquetas , Glicoproteínas da Membrana de Plaquetas/antagonistas & inibidores , Receptores Acoplados a Proteínas G/antagonistas & inibidores , Animais , Humanos , Plantas
7.
Zhongguo Zhong Yao Za Zhi ; 43(7): 1404-1409, 2018 Apr.
Artigo em Zh | MEDLINE | ID: mdl-29728029

RESUMO

Ginkgo diterpene lactone raw material, as a raw material for ginkgo diterpene lactone meglumine injection, is extracted and purified from ginkgo leaf. ¹H-NMR content determination method and fingerprint analysis method were respectively established for ginkgo diterpene lactone raw material. Content determination was conducted in 3 batches of samples by using ¹H-qNMR, and then the results were basically consistent with the results in HPLC method. Twenty-four proton peaks were identified as common fingerprint peaks, and the fingerprint peaks were identified by using the control product and NMR information. Furthermore, 10 batches of samples were analyzed by ¹H-NMR fingerprint. The similarities were all higher than 0.99 and the common peaks were identified with the reference standards. This method is easy, fast, with good precision, stability and repeatability and could provide basis and new ideas for quality evaluation of ginkgo diterpene lactone raw material and its preparations.


Assuntos
Diterpenos/análise , Ginkgo biloba/química , Lactonas/análise , Cromatografia Líquida de Alta Pressão , Medicamentos de Ervas Chinesas/análise , Espectroscopia de Prótons por Ressonância Magnética , Controle de Qualidade
8.
Zhongguo Zhong Yao Za Zhi ; 43(22): 4439-4449, 2018 Nov.
Artigo em Zh | MEDLINE | ID: mdl-30593236

RESUMO

To analyze and identify the chemical components in Xingbei Zhike Keli by using ultra-performance liquid chromatography-quadrupole-time of flight mass spectrometry (UPLC-Q-TOF-MS/MS). The analysis was performed on Agilent Zorbax SB-C18(4.6 mm×250 mm, 5 µm) column, with methanol-0.08% formic acid solution (including 0.1% ammonium formate) as the mobile phase for gradient elution. The flow rate was 1 mL·min⁻¹ and column temperature was 30 °C. The MS spectrum was acquired in both negative and positive ion modes by using electron spray ionization (ESI). These components were further analyzed based on accurate m/z, secondary fragmentation and other information combined with reference substance and literature data. As a result, 87 compounds were successfully identified and predicted, including alkaloids, flavonoids, coumarins and saponins, of which 23 compounds were verified by comparing with reference substances. These results provide reference for the quality control of Xingbei Zhike Keli, and lay the foundation for elucidating their effective components and mechanism of action.


Assuntos
Medicamentos de Ervas Chinesas , Alcaloides , Cromatografia Líquida de Alta Pressão , Flavonoides , Espectrometria de Massas por Ionização por Electrospray , Espectrometria de Massas em Tandem
9.
Zhongguo Zhong Yao Za Zhi ; 43(7): 1384-1391, 2018 Apr.
Artigo em Zh | MEDLINE | ID: mdl-29728027

RESUMO

Ginkgo terpene lactones, as an important active ingredient from Ginkgo leaves, has high medicinal values and has been widely used in clinics. This article would review the researches both at home and abroad, including chemical composition, structure-activity relationship, analytical methods, pharmacological effects, pharmacokinetic characteristics, and so on, providing a reference for further development and utilization of ginkgo terpene lactones.


Assuntos
Ginkgo biloba/química , Lactonas/química , Folhas de Planta/química , Terpenos/química , Medicamentos de Ervas Chinesas/química , Medicamentos de Ervas Chinesas/farmacologia , Lactonas/farmacologia , Terpenos/farmacologia
10.
Zhongguo Zhong Yao Za Zhi ; 43(10): 2118-2122, 2018 May.
Artigo em Zh | MEDLINE | ID: mdl-29933680

RESUMO

Focal cerebral ischemia reperfusion is an essential process during ischemic stroke. The apoptosis of vascular endothelial cells induced by ischemia/reperfusion (I/R) injury is an important cause for brain injury after focal cerebral ischemia. Longxuetongluo capsule (LTC) has been used for the treatment of ischemic stroke in clinic. However, its underlying action mechanism is still unclear. This study aimed to verify the protective effect and mechanisms of LTC on HUVEC cells against oxygen-glucose deprivation/reoxygenation (OGD/R) injury through MTT, LDH, flow cytometry, AO/EB staining and western blot assays. As a result, OGD/R significantly decreased the viability of HUVEC cells, which was significantly improved by LTC. LDH release assay showed that OGD/R significantly increased the lactate dehydrogenase (LDH) release, and LTC dramatically reduced the OGD/R-induced LDH release. Further mechanism study indicated that LTC dose-dependently inhibited the cleavage of PARP, caspase 3, and caspase 9 induced by OGD/R, suggesting that LTC could inhibit the activation of caspase 3/9 apoptosis pathway in the OGD/R-induced apoptosis of HUVEC cells. In conclusion, LTC could protect HUVEC cells against OGD/R injury by inhibiting the activation of mitochondria-related caspase 3/9 apoptosis pathway.


Assuntos
Apoptose/efeitos dos fármacos , Medicamentos de Ervas Chinesas/farmacologia , Células Endoteliais/efeitos dos fármacos , Traumatismo por Reperfusão , Sobrevivência Celular , Glucose , Humanos , Oxigênio
11.
Zhongguo Zhong Yao Za Zhi ; 43(6): 1241-1246, 2018 Mar.
Artigo em Zh | MEDLINE | ID: mdl-29676135

RESUMO

To observe the protective effect of Longxue Tongluo capsule (LTC) on human umbilical vein endothelial cells (EAhy.926 cells) injury induced by oxidized low-density lipoprotein (ox-LDL, 100 mg·L⁻¹). The effect of the cell viability of LTCin alleviating OX-LDL-induced endothelial cell injury was determined by MTT and LDH assay. The effect of LTC on lactic dehydrogenase (LDH), nitric oxide (NO), super oxide dlsmutase (SOD) and malondialdehyde (MDA) levels were detected by corresponding assay kits according to manufacturer's instruction. The effect of LTC on the protein expressions of intercellular cell adhesion molecule-1 (ICAM-1), vascular cell adhesion molecule 1 (VCAM-1), p65, p-p65, IKB and p-IKB were detected by Western blot. The results showed that compared with the normal control group, the activity of EAhy.926 cells was significantly decreased, LDH leakage (P<0.01) increased, NO content and SOD activity significantly decreased (P<0.01, P<0.05), and the expressions of ICAM-1, VCAM-1, p-p65/p65 and p-IKB(P<0.05)increased.This study demonstrated that LTC had no significant effect on the growth of normal cells. The treatment with LTC significantly promoted the proliferation of vascular endothelial cells damagedby ox-LDL, decreased MDA content and LDH release, andincreased the activity of SOD and NO content. Meanwhile, ox-LDL significantly increased the expressions of ICAM-1, VCAM-1, p-p65/p65, p-IKB/IKB in Eahy.926 cells; these effects were suppressed by LTC at 1, 2 mg·L⁻¹. In conclusion, LTC has a significant protective effect on human umbilical vein endothelial cells caused by ox-LDL. This study suggested that LTC has a certain therapeutic effect on AS.


Assuntos
Medicamentos de Ervas Chinesas/farmacologia , Células Endoteliais da Veia Umbilical Humana/efeitos dos fármacos , Lipoproteínas LDL/efeitos adversos , Estresse Oxidativo , Células Cultivadas , Humanos , L-Lactato Desidrogenase/metabolismo , Malondialdeído/metabolismo , Óxido Nítrico/metabolismo , Superóxido Dismutase/metabolismo
12.
Zhongguo Zhong Yao Za Zhi ; 43(7): 1467-1470, 2018 Apr.
Artigo em Zh | MEDLINE | ID: mdl-29728038

RESUMO

A new compound(Z)-6-hydroxy-4-methoxy-5,7-dimethylaurone was isolated from Cleistocalyx operculatus flower buds. Its structure was identified by spectroscopic data including MS, ¹H-NMR, ¹³C-NMR HSQC and HMBC. A known compound, 2',4'-dihydroxy-6'-methoxy-3'5'-dimethylchalcone (DMC), was also isolated and identified,and used as material to synthesize (Z)-6-hydroxy-4-methoxy-5,7-dimethylaurone.Anti-inflammatory activities of the two compounds were tested in vitro. The results showed that (Z)-6-hydroxy-4-methoxy-5,7-dimethylaurone possesses much stronger PGE2 inhibitory activity (IC50 6.12 nmol·L⁻¹) than the positive control ibuprofen (68.66 nmol·L⁻¹ï¼‰.


Assuntos
Anti-Inflamatórios/farmacologia , Benzofuranos/farmacologia , Flores/química , Syzygium/química , Anti-Inflamatórios/isolamento & purificação , Benzofuranos/isolamento & purificação , Chalconas , Dinoprostona/antagonistas & inibidores
13.
Biomed Chromatogr ; 31(6)2017 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-27862112

RESUMO

In this work, a sensitive and efficient method was established and validated for qualitative and quantitative analysis of major bioactive constituents in Dazhu Hongjingtian capsule by liquid chromatography tandem mass spectrometry. A total of 32 compounds were tentatively identified using ultra-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry. Furthermore, 12 constituents, namely gallic acid, 3,4-dihydroxybenzoic acid, salidroside, p-coumaric acid-4-O-ß-d-glucopyranoside, bergeninum, 4-hydroxybenzoic acid, 4-hydroxyphenylacetic acid, syringate, 6''-O-galloylsalidroside, rhodiosin, rhodionin and kaempferol-7-O-α-l-rhamnoside, were simultaneously quantified by the developed ultra-performance liquid chromatography coupled with a triple quadrupole mass spectrometry method in 9 min. All of them were analyzed on an Agilent ZorBax SB-C18 column (3.0 × 100 mm, 1.8 µm) with linear gradient elution of methanol-0.1% formic acid water. The proposed method was applied to analyze three batches of samples with acceptable linearity (R, 0.9979-0.9997), precision (RSD, 1.3-4.7%), repeatability (RSD, 1.7-4.9%), stability (RSD, 2.2-4.9%) and recovery (RSD, 0.6-4.4%) of the 12 compounds. As a result, the analytical method possessing high throughput and sensitivity is suitable for the quality control of Dazhu Hongjingtian capsule.


Assuntos
Cromatografia Líquida/métodos , Medicamentos de Ervas Chinesas/química , Espectrometria de Massas em Tandem/métodos , Padrões de Referência , Reprodutibilidade dos Testes
14.
Biomed Chromatogr ; 31(12)2017 Dec.
Artigo em Inglês | MEDLINE | ID: mdl-28543360

RESUMO

Daphne genkwa Sieb.et Zucc. is a well-known medicinal plant. This study was designed to apply the ultra-high performance liquid chromatography system to establish a quality control method for D. genkwa. Data revealed that there were 15 common peaks in 10 batches of D. genkwa Sieb. Et Zucc. (Thymelaeaceae) from different provinces of China. On this basis, the fingerprint chromatogram was established to provide references for quality control. Afterwards, the chemical constitutions of these common peaks were analyzed using the UPLC-Q-TOF-MS system and nine of them were identified. In addition, LPS-stimulated RAW264.7 murine macrophages and DPPH assay were used to study the anti-inflammatory and anti-oxidation effects of D. genkwa. Then the fingerprint-efficacy relationships between UPLC fingerprints and pharmacodynamic data were studied with canonical correlation analysis. Analysis results indicated that the anti-inflammatory and anti-oxidation effects differed among the 10 D. genkwa samples owing to their inherent differences of chemical compositions. Taken together, this research established a fingerprint-efficacy relationship model of D. genkwa plant by combining the UPLC analytic technique and pharmacological research, which provided references for the detection of the principal components of traditional Chinese medicine on bioactivity.


Assuntos
Anti-Inflamatórios/química , Antioxidantes/química , Cromatografia Líquida de Alta Pressão/métodos , Daphne/química , Espectrometria de Massas/métodos , Extratos Vegetais/química , Animais , Anti-Inflamatórios/farmacologia , Antioxidantes/farmacologia , Compostos de Bifenilo/análise , Compostos de Bifenilo/metabolismo , Macrófagos/efeitos dos fármacos , Macrófagos/metabolismo , Camundongos , Óxido Nítrico/análise , Óxido Nítrico/metabolismo , Picratos/análise , Picratos/metabolismo , Extratos Vegetais/farmacologia , Células RAW 264.7 , Reprodutibilidade dos Testes
15.
Zhongguo Zhong Yao Za Zhi ; 42(17): 3368-3373, 2017 Sep.
Artigo em Zh | MEDLINE | ID: mdl-29192448

RESUMO

To establish a UPLC-MS/MS method for simultaneous determination of six triterpenoid constituents (pachymic acid, dehydropachymic acid, dehydrotumulosic acid, polyporenic acid C, dehydroeburicoic acid and dehydrotra metenolic acid) in Guizhi Fuling capsules (GFC). Chromatographic analysis was conducted on Agilent Porosheell 120 SB-C18 column (4.6 mm×150 mm, 2.7 µm), with 0.1% formic acid aqueous solution-methanol as the mobile phase for gradient elution at a flow rate of 0.4 mL•min-1. The column temperature was 30 ℃ and the sample size was 5 µL. The samples were analyzed by tandem mass spectrometer with negative electrospray ionization (ESI) source, and monitored under a multiple reaction monitoring (MRM) mode, with the quantitative ion pairs m/z 527.8→465.5 (pachymic acid), m/z 525.6→465.6 (dehydropachymic acid), m/z 483.4→337.3 (dehydrotumulosic acid), m/z 481.5→419.5 (polyporenic acid C), m/z 467.4→337.1 (dehydroeburicoic acid), m/z 453.4→337.0 (dehydrotra metenolic acid). Six triterpenoid acids showed good linear relationships within the investigated concentration ranges (r> 0.996 8), with RSDs of precision less than 6.2%, and all RSDs of repeatability less than 5.9%. The average recovery rate was 97.90%, 100.2%, 99.60%, 101.7%, 102.6% and 103.0% respectively. The method was rapid, accurate, repeatable and could be used as a method for quantitative determination of triterpenoid acids in Chinese medicine prescriptions, providing a reference method for the quality control of Guizhi Fuling capsules and providing a reference for the content determination for Chinese medicine prescriptions containing Poria cocos.


Assuntos
Medicamentos de Ervas Chinesas/química , Compostos Fitoquímicos/análise , Triterpenos/análise , Wolfiporia/classificação , Cápsulas , Cromatografia Líquida de Alta Pressão , Espectrometria de Massas por Ionização por Electrospray , Espectrometria de Massas em Tandem
16.
Zhongguo Zhong Yao Za Zhi ; 42(18): 3546-3552, 2017 Sep.
Artigo em Zh | MEDLINE | ID: mdl-29218940

RESUMO

The "design space" method was used to optimize the purification process of Resina Draconis phenol extracts by using the concept of "quality derived from design" (QbD). The content and transfer rate of laurin B and 7,4'-dihydroxyflavone and yield of extract were selected as the critical quality attributes (CQA). Plackett-Burman design showed that the critical process parameters (CPP) were concentration of alkali, the amount of alkali and the temperature of alkali dissolution. Then the Box-Behnken design was used to establish the mathematical model between CQA and CPP. The variance analysis results showed that the P values of the five models were less than 0.05 and the mismatch values were all greater than 0.05, indicating that the model could well describe the relationship between CQA and CPP. Finally, the control limits of the above 5 indicators (content and transfer rate of laurine B and 7,4'-dihydroxyflavone, as well as the extract yield) were set, and then the probability-based design space was calculated by Monte Carlo simulation and verified. The results of the design space validation showed that the optimized purification method can ensure the stability of the Resina Draconis phenol extracts refining process, which would help to improve the quality uniformity between batches of phenol extracts and provide data support for production automation control.


Assuntos
Croton/química , Medicamentos de Ervas Chinesas/análise , Extratos Vegetais/análise , Resinas Vegetais/análise , Tecnologia Farmacêutica , Modelos Teóricos , Método de Monte Carlo , Fenóis
17.
Zhongguo Zhong Yao Za Zhi ; 42(18): 3537-3545, 2017 Sep.
Artigo em Zh | MEDLINE | ID: mdl-29218939

RESUMO

To investigate the effect of hot air circulation drying and spray drying on the quality of Tianshu capsule from the view point of chemical compositions. UPLC-DAD was used to establish the fingerprint of Tianshu capsules for the first time, and the main chemical constituents were identified by UPLC-Q-TOF-MS/MS. A total of 62 compounds were identified in this method, 21 of which were reported in Tianshu capsules for the first time. The results showed that there were no significant differences in the identification of the chemical constituents types between these two methods, but the contents of some constituents were different. The common patterns generated by the 10 batches of hot air cycle drying samples were used as the control fingerprint, and the similarity of the spray drying samples fingerprints was 0.877, with high similarity of the fingerprints between these two methods. UPLC-DAD combined with UPLC-Q-TOF-MS/MS technology was used for the first time to evaluate the chemical constituents of Tianshu capsule rapidly, comprehensively and accurately, providing technical support for the quality evaluation of Tianshu capsule.


Assuntos
Dessecação/métodos , Medicamentos de Ervas Chinesas/química , Tecnologia Farmacêutica/métodos , Cromatografia Líquida de Alta Pressão , Controle de Qualidade , Espectrometria de Massas em Tandem
18.
Zhongguo Zhong Yao Za Zhi ; 42(5): 931-935, 2017 Mar.
Artigo em Zh | MEDLINE | ID: mdl-28994537

RESUMO

To study Ginkgo biloba leaves in different producing area, we establish an HPLC method for the simultaneously determination of seven flavonoids glycosides and four biflavonoids in G. biloba leaves. The analysis was performed on an Agilent ZORBAX SB-C18 column(4.6 mm×250 mm, 5 µm) wich acetonitrile, and 0.4% phosphoric acid as mobile phase at flow rate of 1 mL•min⁻¹ in a gradient edution, and the detection was carried out at 254 nm.The calibration curves of the seven flavonoids glycosides and four biflavonoids had a good linearitiy with good recoveries. The established HPLC method is simple, rapid, accurate, reliable, and sensitive, and can be applied to the identification and quality control of G. biloba leaves.


Assuntos
Flavonoides/isolamento & purificação , Ginkgo biloba/química , Glicosídeos/isolamento & purificação , Folhas de Planta/química , Cromatografia Líquida de Alta Pressão
19.
Zhongguo Zhong Yao Za Zhi ; 42(10): 1901-1907, 2017 May.
Artigo em Zh | MEDLINE | ID: mdl-29090549

RESUMO

The aim of this study was to develop a simple, sensitive ultra performance liquid chromatography mass spectrometry (UPLC-MS/MS) method for the determination of syringaresinol, N-trans-feruloyltyramine, chelerythrine chloride, sinomenine, coptisine chloride, sanguinarine, chelidonine, magnolflorine, allocryptopine, protopine, farrerol, stylopine and dihydrosanguin-arine in Tong'an injection (TAI), which could be used for the quality control of TAI. The UPLC analysis was performed on Agilent Zorbax SB-Aq column (2.1 mm×150 mm,3.5 µm), with 0.1% formic acid solution (A) -acetonitrile (B) as the mobile phase for gradient elution (0.01-2 min, 5%B; 2-8 min, 5%-30%B; 8-11 min, 30%-95%B; 11-13 min, 95%B; 13-13.1 min, 95%-5%B; 13.1-14 min, 5%B). The flow rate was 0.5 mL•min⁻¹, and the column temperature was 25 ℃; multiple reaction monitoring (MRM) was performed in electrospray ion source positive ion mode for quantitative determination. The calibration curves for the above thirteen compounds showed good linear relationship in corresponding mass concentration range (r>0.999 0). The average recovery rate of the compounds ranged from 95.70% to 104.8%, with RSD of less than 1.9%. The contents of thirteen active components in 10 batches of TAI were 0.021 2-0.029 0, 0.001 7-0.002 3, 0.000 9-0.001 3, 5.952-6.205 2, 0.195 4-0.240 5, 0.002 0-0.002 9, 0.693-0.798 2, 0.069 3-0.078 2, 0.089 29-0.102 9, 0.386 5-0.420 1, 0.014 3-0.015 9, 0.755 3-0.842 1, and 0.008 2-0.011 2 g•L⁻¹ respectively. Methodology validation proved that this method was simple, rapid, sensitive and accurate, which can be used to provide reference for the comprehensive evaluation of TAI quality. The determination results of 10 batches of TAI showed the content of each batch had no significant difference. The results may provide a basis for the quality control of TAI.


Assuntos
Cromatografia Líquida de Alta Pressão , Medicamentos de Ervas Chinesas/análise , Compostos Fitoquímicos/análise , Espectrometria de Massas em Tandem , Controle de Qualidade , Reprodutibilidade dos Testes
20.
Biomed Chromatogr ; 30(2): 131-41, 2016 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-26058547

RESUMO

A high-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (HPLC/Q-TOF MS) was developed for the analysis of chemical composition change in the production process of Re Du Ning injection, a Chinese medicine preparation with a combination of Lonicera japonica Thunb., Gardenia jasminoides Ellis and Artemisia annua L. A total of 90 compounds from raw materials-intermediates-Re Du Ning injection were detected; among them, 55 compounds were identified or tentatively characterized, and the characteristic ions of different types of compounds were described. Based on these studies, the different types of compounds in the various process routes were analyzed. A total of 28 compounds, including seven iridoid glycosides and six monoterpenes from G. jasminoides Ellis, five iridoid glycosides, nine phenolic acids and one unknown compound from L. japonica Thunb., were transferred to Re Du Ning injection, and two unknown compounds were generated in the production process of Re Du Ning injection. The results indicated that the Chinese Medicine Pharmaceutical process control is very important. This method could provide some reference for other Chinese medicine preparations.


Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Medicamentos de Ervas Chinesas/análise , Medicamentos de Ervas Chinesas/química , Espectrometria de Massas por Ionização por Electrospray/métodos , Glicosídeos Iridoides/análise , Glicosídeos Iridoides/química , Fenóis/análise , Fenóis/química , Terpenos/análise , Terpenos/química
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