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1.
Mater Sci Eng C Mater Biol Appl ; 128: 112326, 2021 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-34474877

RESUMO

Bone defects remain a challenging problem for doctors and patients in clinical practice. Processed pyritum is a traditional Chinese medicine that is often used to clinically treat bone fractures. It contains mainly Fe, Zn, Cu, Mn, and other elements. In this study, we added the extract of processed pyritum to ß-tricalcium phosphate and produced a porous composite TPP (TCP/processed pyritum) scaffold using digital light processing (DLP) 3D printing technology. Scanning electron microscopy (SEM) analysis revealed that TPP scaffolds contained interconnected pore structures. When compared with TCP scaffolds (1.35 ± 0.15 MPa), TPP scaffolds (5.50 ± 0.24 MPa) have stronger mechanical strength and can effectively induce osteoblast proliferation, differentiation, and mineralization in vitro. Meanwhile, the in vivo study showed that the TPP scaffold had better osteogenic capacity than the TCP scaffold. Furthermore, the TPP scaffold had good biosafety after implantation. In summary, the TPP scaffold is a promising biomaterial for the clinical treatment of bone defects.


Assuntos
Fosfatos de Cálcio , Tecidos Suporte , Humanos , Porosidade , Impressão Tridimensional
2.
J Anal Methods Chem ; 2021: 6625929, 2021.
Artigo em Inglês | MEDLINE | ID: mdl-33936837

RESUMO

As a popular fermented condiment in oriental countries, soy sauce plays a more and more important role in modern food culture due to its unique smell and delicious taste. With the help of microwave extraction and gas chromatography-tandem mass spectrometry, the sample preparation method is aimed to determine the content of cyclohexane, benzene, toluene, chlorobenzene, and styrene in soy sauce. The method was validated by examining the linearity, accuracy, specificity, precision, the limit of detection, and quantitation. Meanwhile, three key factors have an impact on the efficiency and accuracy of the method including extracting solvent, temperature, and time which were optimized. The result shows that the recoveries of spiked analytes ranged from 80.86% to 105.71%, the relative standard deviation of intraday and interday precision was no more than 12.1% and 12.5%, and the limit of detection and quantitation were 0.25-1.00 ng/mL and 0.50-2.00 ng/mL, respectively. The results also indicated that the proposed method was a simple, reliable, and sensitive approach for the determination trace amount of five harmful volatile organic compounds from soy sauce.

3.
Xenobiotica ; 51(3): 355-365, 2021 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-33269993

RESUMO

Gefitinib, the first approved inhibitor for oral epidermal growth factor receptor (EGFR), has been proved to be effective in non-small cell lung cancer with EGFR mutation. However, there are many metabolites of gefitinib that have not been identified in vivo. This study aims to identify the metabolites of gefitinib and its metabolic pathways in rats using ultra-high-performance liquid chromatography coupled with a quadrupole time-of-flight mass spectrometry (UHPLC-Q-TOF-MS/MS) detector. Protein precipitation, solid-phase and ultrasonic extraction were used for the pre-treatment of plasma, urine, bile and faeces samples. In this study, a total of 28 compounds were identified in rat plasma, 29 in bile, 20 in urine and 16 in faeces. 20 new compounds were firstly reported as metabolites of gefitinib. Reduction, hydroxylation, dealkylation and dehalogenation were the major metabolic pathways in phase I. For phase II, the main pathways were sulphate and glucuronide conjugation. The fragment ions of gefitinib and its metabolites were usually generated via the fracture of C1-O bond of propoxy on the C6 position of aniline quinazoline ring. The results may be valuable and important for understanding the metabolic process of gefitinib in clinical application and drug safety.


Assuntos
Antineoplásicos/metabolismo , Gefitinibe/metabolismo , Redes e Vias Metabólicas , Animais , Bile/química , Cromatografia Líquida de Alta Pressão , Fezes/química , Plasma/química , Ratos , Ratos Sprague-Dawley , Espectrometria de Massas em Tandem , Urina/química
4.
J Chromatogr Sci ; 59(2): 182-190, 2021 Jan 14.
Artigo em Inglês | MEDLINE | ID: mdl-33173942

RESUMO

BACKGROUND: A simple, rapid and sensitive method coupling ultrasound-assisted dispersive liquid-liquid microextraction (DLLME) with ultra-high performance liquid chromatography-tandem mass spectrometry was developed for the simultaneous determination of malachite green (MG) and crystal violet (CV) in different water samples. OBJECTIVE: In ultrasound-assisted DLLME procedure, several parameters affecting the extraction efficiency, including pH, type and volume of the extraction and dispersive solvents, extraction time, ionic strength, were optimized to improve the accuracy and precision of this method. METHODS: MG and CV were extracted and preconcentrated using dichloromethane and acetonitrile as the extraction and dispersive solvents, respectively. RESULTS: Under the optimum conditions, the proposed method affords good linearity in the range of 0.40-20.0 ng/L, and the limit of detections were 0.21 and 0.32 ng/L for MG and CV, respectively. The recoveries of the method at three spiked levels were in the range of 83.4-94.2% with relative standard deviations lower than 4.7% (n = 3). CONCLUSIONS: Satisfactorily, no significant matrix effect has been found as the data ranged between 68% and 102%.


Assuntos
Antibacterianos , Microextração em Fase Líquida/métodos , Antibacterianos/análise , Antibacterianos/química , Antibacterianos/isolamento & purificação , Cromatografia Líquida de Alta Pressão/métodos , Limite de Detecção , Modelos Lineares , Reprodutibilidade dos Testes , Sonicação , Espectrometria de Massas em Tandem/métodos
5.
Chin J Nat Med ; 18(12): 916-921, 2020 Dec.
Artigo em Inglês | MEDLINE | ID: mdl-33357722

RESUMO

In the present study, liquiritigenin-phospholipid complex (LPC) was developed and evaluated to increase the oral bioavailability of liquiritigenin. A single-factor test methodology was applied to optimize the formulation and process for preparing LPC. The effects of solvent, drug concentration, reaction time, temperature and drug-to-phospholipid ratio on encapsulation efficiency were investigated. LPCs were characterized by UV-visible spectroscopy, differential scanning calorimetry (DSC), fourier transform infrared spectroscopy (FTIR), and powder X-ray diffractometry (PXRD). The apparent solubility and n-octanol/water partition coefficient were tested. The pharmacokinetic characteristics and bioavailability of the LPC were investigated after oral administration in rats in comparison with liquiritigenin alone. An LPC was successfully prepared. The optimum level of various parameters for liquiritigenin-phospholipid complex was obtained at the drug concentration of 8 mg·mL-1, reaction time for 15 min, reaction temperature of 30 ℃, a ratio of 1∶4.5 (W/W) drug-to-phospholipid and anhydrous ethanol as reaction solvent. Compared to liquiritigenin, the AUC0-t of the LPC was increased by 239%. The liquiritigenin-phospholipid complex significantly increase the lipid solubility and bioavailability of liquiritigenin, suggesting that it is an effective formulation for further development and clinical applications.


Assuntos
Flavanonas/farmacocinética , Fosfolipídeos/farmacocinética , Administração Oral , Animais , Disponibilidade Biológica , Ratos , Solventes
6.
Int J Anal Chem ; 2020: 9760580, 2020.
Artigo em Inglês | MEDLINE | ID: mdl-32952560

RESUMO

A simple, sensitive, and exact methyl esterification in combination with gas chromatography-mass spectrometry (GC-MS) method was developed to determine the contents of palmitic acid and stearic acid in the chlorinated butyl rubber stoppers and liposome injections in order to evaluate the compatibility of pharmaceutical packaging materials. In this experiment, palmitic acid and stearic acid were detected in the form of methyl hexadecanoate and methyl stearate in chlorinated butyl rubber stoppers and liposome injections. The results showed good linearities in the range of 0.50-10.00 µg·mL-1 for methyl hexadecanoate and 1.00-20.00 µg·mL-1 for methyl stearate, with the limits of detection (LOD) 11.94 ng·mL-1 and 11.90 ng·mL-1, respectively. The recoveries that ranged from 95.25% to 100.29% were satisfied, and the relative standard deviation (RSD) was no more than 7.16%. The developed method was successfully applied to evaluate the compatibility of chlorinated butyl rubber stoppers with liposome injections and the safety assessment.

7.
Artigo em Inglês | MEDLINE | ID: mdl-32526664

RESUMO

Dahuang zhechong pill (DHZCP) is a famous traditional Chinese medicine prescription, which is widely used in the treatment of liver diseases. However, due to the lack of a dynamic DHZCP profile, the in vivo pharmacokinetics of active ingredients within this medicine remains unknown. In this paper, a rapid, sensitive and reliable UHPLC-MS/MS method was used to determine the content of 19 characteristic constituents of DHZCP in rat plasma, including rhein, emodin, chrysophanol, physcion, aloeemodin, p-methoxyphenylacetic acid, hypoxanthine nucleoside, wogonin, wogonoside, baicalin, norwogonin, naringenin, nutmeg acid, paeoniflorin, verbascoside, rhodiola glucoside, forsythoside A, formononetin, and glycyrrhizic acid. An Agilent Extend-C18 column (2.1 mm × 100 mm, 1.8 µm) was used to separate the 19 characteristic constituents, with a mobile phrase of (A) 0.1% formic acid and (B) acetonitrile. The constituents were detected in negative ion mode with multiple reactions monitoring (MRM). The established UHPLC-MS/MS method had good linearity, with a coefficient of determination (r2) of >0.99. The daytime and intra-day precision were less than 12%, and the accuracy ranged from -9.56% to 7.82%. The stability, extraction recovery, and matrix effect met the requirements. The method was successfully applied to the pharmacokinetic study of these nineteen characteristic constituents after oral administration of DHZCP. UHPLC-MS/MS was used for the first time to study the pharmacokinetics of the characteristic chemical constituents in DHZCP, which provided reference and theoretical guidance for further clarification of its pharmacodynamic basis.

8.
Zhongguo Zhong Yao Za Zhi ; 45(5): 1135-1141, 2020 Mar.
Artigo em Chinês | MEDLINE | ID: mdl-32237457

RESUMO

There are many chemical components in the volatile oil of Dictamni Cortex. The complex network relationship of "component-target-disease" can be revealed by using the network pharmacology method, and the mechanism of the efficacy of Dictamni Cortex can be revealed. In this study, we used Swiss Target Prediction database to predict the target of action, STRING database to build protein interaction network, and Cytoscape software to build "component-target-disease" network. The results showed that the antibacterial, anti-inflammatory and antiallergic effects of Dictamni Cortex were closely related to the components of thymol methyl ether, elemenol, anethole, and the related targets of each component were cross-linked to play a multi-target pharmacodynamic role. This study laid a foundation for the study of the effective substance basis and quality control evaluation of the Dictamni Cortex, and provided a scientific basis for further revealing its mechanism.


Assuntos
Dictamnus/química , Medicamentos de Ervas Chinesas/farmacologia , Óleos Voláteis/farmacologia , Mapas de Interação de Proteínas , Controle de Qualidade , Software
9.
Int J Nanomedicine ; 15: 1101-1115, 2020.
Artigo em Inglês | MEDLINE | ID: mdl-32110010

RESUMO

Background: The clinical use of doxorubicin (DOX) is severely limited due to its cardiotoxicity. Thus, there is a need for prophylactic and treatment strategies against DOX-induced cardiotoxicity. Purpose: The purpose of this study was to develop a liquiritigenin-loaded submicron emulsion (Lq-SE) with enhanced oral bioavailability and to explore its efficacy against DOX-induced cardiotoxicity. Methods: Lq-SE was prepared using high-pressure homogenization and characterized using several analytical techniques. The formulation was optimized by central composite design response surface methodology (CCD-RSM). In vivo pharmacokinetic studies, biochemical analyses, reactive oxygen species (ROS) assays, histopathologic assays, and Western blot analyses were performed. Results: Each Lq-SE droplet had a mean particle size of 221.7 ± 5.80 nm, a polydispersity index (PDI) of 0.106 ± 0.068 and a zeta potential of -28.23 ± 0.42 mV. The area under the curve (AUC) of Lq-SE was 595% higher than that of liquiritigenin (Lq). Lq-SE decreased the release of serum cardiac enzymes and ameliorated histopathological changes in the hearts of DOX-challenged mice. Lq-SE significantly reduced oxidative stress by adjusting the levels of ROS, increasing the activity of antioxidative enzymes and inhibiting the protein expression of NOX4 and NOX2. Furthermore, Lq-SE significantly improved the inflammatory response through the mitogen-activated protein kinase (MAPK)/nuclear factor-κB (NF-κB) signalling pathway and induced cardiomyocyte apoptosis. Conclusion: Lq-SE could be used as an effective cardioprotective agent against DOX in chemotherapy to enable better treatment outcomes.


Assuntos
Cardiotoxicidade/prevenção & controle , Doxorrubicina/efeitos adversos , Emulsões/química , Flavanonas/farmacologia , Administração Oral , Animais , Anti-Inflamatórios/farmacologia , Antioxidantes/metabolismo , Antioxidantes/farmacologia , Apoptose/efeitos dos fármacos , Disponibilidade Biológica , Cardiotônicos/farmacologia , Cardiotoxicidade/metabolismo , Emulsões/administração & dosagem , Feminino , Flavanonas/administração & dosagem , Flavanonas/farmacocinética , Coração/efeitos dos fármacos , Masculino , Camundongos Endogâmicos C57BL , Camundongos Nus , Miocárdio/metabolismo , Miocárdio/patologia , NF-kappa B/metabolismo , Estresse Oxidativo/efeitos dos fármacos , Ratos Sprague-Dawley , Espécies Reativas de Oxigênio/metabolismo
10.
Pharm Biol ; 57(1): 363-368, 2019 Dec.
Artigo em Inglês | MEDLINE | ID: mdl-31295042

RESUMO

Context: The dried fruits of Arctium lappa L. have been used in two forms in traditional Chinese medicine; crude and stir-heating Fructus Arctii. However, its processed product possesses better activity. Objective: In this study, the chemical constituents of both crude and processed Fructus Arctii and their antiproliferative activities were evaluated. Materials and methods: The seven main active components in crude and various processed Fructus Arctii were quantitatively determined using high-performance liquid chromatography (HPLC). According to the actual amount in crude and five processed samples, seven single components were combined as multi-component combinations with six different proportions. The antiproliferative activities of these compatibility component groups were examined using the CCK-8 assay. Results: During the heating process, the proportion of the seven main components changed dynamically. The contents of 3-caffeoylquinic acid (3-CQA), 3,5-dicaffeoylquinic acid (3,5-diCQA), and arctiin (ARC) declined, while the contents of 4-caffeoylquinic acid (4-CQA), 3,4-dicaffeoylquinic acid (3,4-diCQA), 4,5-dicaffeoylquinic acid (4,5-diCQA), and arctigenin (ARG) increased very significantly. Discussion and conclusions: The results also indicated that seven components in the processed samples had higher cytotoxic profiles against HL-60 cells than those in the crude sample. Therefore, the heating process may enhance the antitumor activity of Fructus Arctii by changing the proportion of active components.


Assuntos
Arctium/química , Proliferação de Células/efeitos dos fármacos , Medicamentos de Ervas Chinesas/química , Medicamentos de Ervas Chinesas/farmacologia , Ácido Clorogênico/análogos & derivados , Cromatografia Líquida de Alta Pressão , Frutas/química , Furanos , Glucosídeos , Células HL-60 , Humanos , Lignanas , Medicina Tradicional Chinesa , Ácido Quínico/análogos & derivados
11.
J Sep Sci ; 42(14): 2341-2350, 2019 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-31037812

RESUMO

In China, Semen Cassiae has long been used to protect liver, brighten eyes, and relieve constipation. Prepared Semen Cassiae is produced from raw Semen Cassiae by processing, the two forms of Semen Cassiae have different clinical applications. Pathological state is an important factor affecting the efficacy of drugs, the pharmacokinetic behavior of drugs could be significantly changed when people or animal were under different pathological state. To clarify the effect of processing mechanism and pathological state for pharmacokinetic behavior, the pharmacokinetics of nine components of raw and prepared Semen Cassiae under normal and acute liver injury rats were examined. The results showed that the bimodal phenomenon appeared on the plasma concentration-time profiles of obtusin, emodin, chrysophanol, aloe emodin and rhein. The Tmax of aurantio-obtusin, obtusin, chrysoobtusin, emodin, chrysophanol, aloe emodin, physcion in normal groups administrated prepared Semen Cassiae were shorter than those administrated raw Semen Cassiae. For the AUC0-t , aurantio-obtusin, obtusin, chrysoobtusin, chrysophanol, aloe emodin and physcione in model groups administrated prepared Semen Cassiae were significantly higher than other groups, unlike above components, rhein had poor absorption in model groups. The study would be useful for further studies on pharmacokinetics and clinical application of raw and prepared Semen Cassiae.


Assuntos
Cassia/química , Doença Hepática Induzida por Substâncias e Drogas/sangue , Medicamentos de Ervas Chinesas/farmacocinética , Administração Oral , Animais , Antraquinonas/administração & dosagem , Antraquinonas/sangue , Antraquinonas/farmacocinética , Medicamentos de Ervas Chinesas/administração & dosagem , Emodina/administração & dosagem , Emodina/análogos & derivados , Emodina/sangue , Emodina/farmacocinética , Masculino , Ratos , Ratos Sprague-Dawley
12.
Biomed Chromatogr ; 33(4): e4464, 2019 Apr.
Artigo em Inglês | MEDLINE | ID: mdl-30536751

RESUMO

Xanthii fructus (XF), the fruit of Xanthium sibiricum Patr., is a traditional Chinese materia medica commonly used to treat allergic rhinitis and other rhinitis diseases. To uncover the mechanism of the stir-frying process and its effect on the pharmacokinetic behavior of active compounds in model rats, four active compounds-chlorogenic acid, 4-caffeoylquinic acid, 1,5-O-dicaffeoylquinic acid and apigenin-were selected based on previous spectrum-effect experiments. High performance liquid chromatography tandem triple quadrupole mass spectrometry (UPLC-QqQ-MS) technology, an accurate and feasible method, was applied to measure the concentration of these four compounds in rat plasma. This validated method can accurately measure the concentration of each compound at each sampling point of rat plasma. This validated method shows good linearity, extraction recoveries, matrix effects, intra- and inter-day precision and stabilities. Compared with the XF group, the maximum plasma concentration (Cmax ) value of 1,5-O-dicaffeoylquinic acid decreased remarkably (p < 0.05) after oral administration of stir-fried Xanthii fructus (SXF) extract, while the other compounds showed no significant difference. The mean residence time value of chlorogenic acid (p < 0.05) and 1,5-O-dicaffeoylquinic acid (p<0.01) after oral administration of SXF extraction demonstrated significant differences compared with the XF group, while the other two compounds showed no statistical difference, indicating that the stir-frying process prolonged the effect time and delayed the removal time of chlorogenic acid and 1,5-O-dicaffeoylquinic acid. The values of the area under the plasma concentration-time curve from zero to the last quantifiable time-point, the area under the plasma concentration-time curve from zero to infinity, the time to maximum concentration and the elimination half-life of four compounds in the SXF group showed no statistically significant difference from the XF group. From this data, we speculated that the stir-frying process can not only keep the absorption of 4-caffeoylquinic acid and apigenin, but also increase the effect time of chlorogenic acid and 1,5-O-dicaffeoylquinic acid, which could be the mechanism underlying the stir-frying process enhancing the effects of XF.


Assuntos
Apigenina/sangue , Cromatografia Líquida de Alta Pressão/métodos , Cinamatos/sangue , Medicamentos de Ervas Chinesas/farmacocinética , Espectrometria de Massas em Tandem/métodos , Administração Oral , Animais , Apigenina/química , Apigenina/farmacocinética , Cinamatos/química , Cinamatos/farmacocinética , Estabilidade de Medicamentos , Medicamentos de Ervas Chinesas/administração & dosagem , Medicamentos de Ervas Chinesas/química , Limite de Detecção , Modelos Lineares , Masculino , Ratos , Ratos Sprague-Dawley , Reprodutibilidade dos Testes
13.
Zhonghua Wei Zhong Bing Ji Jiu Yi Xue ; 31(11): 1373-1377, 2019 Nov.
Artigo em Chinês | MEDLINE | ID: mdl-31898568

RESUMO

OBJECTIVE: To investigate the clinical effect of modified Graeb criteria score and Glasgow coma score (GCS) in individualized treatment of intraventricular hemorrhage. METHODS: 113 patients with intraventricular hemorrhage admitted to the department of neurosurgery of Second Affiliated Hospital of Guangxi Medical University from June 2014 to February 2018 were enrolled, and they were divided into 13-15, 9-12, and 3-8 groups according to GCS score at admission, and modified Graeb criteria score was classified as grade I, II and III at the same time. In GCS 9-12 and 3-8 groups, patients with modified Graeb criteria score grade III were treated with bilateral extra ventricular drainage, patients with modified Graeb criteria score grade II were treated with bilateral extra ventricular drainage or lumbar cistern drainage (GCS 9-12 group was more prior to lumbar cistern drainage, 3-8 group was given priority to extra ventricular drainage), and patients with modified Graeb criteria score grade I were treated conservatively. In GCS 13-15 group, bilateral extra ventricular cerebral drainage or lumbar cistern drainage was performed if the modified Graeb criteria score grade was III, lumbar cistern drainage or conservative treatment was performed if the modified Graeb criteria score grade was II, and conservative treatment was performed if the modified Graeb criteria score grade was I. The changes in GCS score at 1 month after individualized treatment and the favourable prognosis rate at 6 months after treatment were observed [favourable prognosis was defined as Glasgow outcome score (GOS) IV-V] as well as the basic clearance time of intraventricular hematomas, and the occurrence of complications such as intracranial infection, pulmonary infection and hydrocephalus were recorded. RESULTS: 113 patients with intraventricular hemorrhage were enrolled in the final analysis, including 39 patients in GCS 13-15 group, 27 in 9-12 group, and 47 in 3-8 group; 21 patients with the first grade of modified Graeb criteria score, 42 with the second grade and 50 with the third grade. At 1 month after individualized treatment, the GCS scores in GCS 13-15 and 9-12 groups were significantly higher than those at admission (14.8±0.2 vs. 13.7±0.8, 13.1±1.7 vs. 10.7±1.1, both P < 0.05). When comparing the GCS score of the same patient at admission with that of 1 month after treatment, the GCS scores of the three groups were significantly improved, indicating that the consciousness of patients with different coma levels at admission had been significantly improved after individualized treatment. The basic clearance time of intracerebroventricular hematomas in patients with the second grade of modified Graeb criteria score was (7.0±2.8) days, in patients with the third grade was (6.1±2.0) days. At 6 months after individualized treatment, among 113 patients, GOS score was grade I in 7 patients (6.2%), grade II in 13 patients (11.5%), grade III in 28 patients (24.8%), grade IV in 27 patients (23.9%), and grade V in 38 patients (33.6%), with the favourable prognosis rate of 57.5% (65/113). Among 113 patients, intracranial infection occurred in 5 patients (4.4%), pulmonary infection in 22 patients (19.5%), hydrocephalus in 2 patients (1.8%) and rebleeding in 4 patients (3.5%). In 83 patients with lumbar cistern drainage, 1 patient had post-drainage infection (1.2%), 3 patients had plugging (3.6%), 6 patients had accidental drop of drainage tube (7.2%), and none of them had occipital macroforamen hernia after drainage. Seven of the 113 patients died including 2 patients died of cerebral hernia caused by rebleeding, 5 patients died of severe pneumonia or automatic discharge from hospital. CONCLUSIONS: The combination of modified Graeb criteria score and GCS score can individualize treatment for patients with intraventricular hemorrhage and effectively improve the prognosis of patients with intraventricular hemorrhage.


Assuntos
Hemorragia Cerebral , Escala de Coma de Glasgow , China , Humanos , Hidrocefalia , Prognóstico , Estudos Retrospectivos , Resultado do Tratamento
14.
Se Pu ; 37(12): 1297-1304, 2019 Dec 08.
Artigo em Chinês | MEDLINE | ID: mdl-34213131

RESUMO

In this work, a method for the determination of the amounts of the four genotoxic impurities in gefitinib has been developed. A simple and sensitive high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) approach has been developed, optimized, and validated. The genotoxic impurities were 3-chloro-4-fluoroaniline, 3,4-difluoroaniline, 3-fluoro-4-chloroaniline, and 3,4-dichloroaniline. Separation was achieved on an Inertsil ODS-3 column (100 mm×3.0 mm, 3 µm). The column temperature was 40 ℃, and the running time was 12 min. A triple quadrupole mass detector with positive electrospray ionization in the multiple reaction monitoring (MRM) mode was applied. The method was validated in terms of its specifi-city, linearity, precision, accuracy, stability, and robustness. The correlation coefficient of each impurity was higher than 0.999 in the range of 0.6-96.0 µg/L. The limits of detection (LODs) and limits of quantity (LOQs) were in the ranges of 0.2-2.0 µg/L and 0.6-6.0 µg/L, respectively. The recoveries of all impurities at 6, 30, and 60 µg/L were within 91.0%-98.5%. All impurities were stable within 2 h. After detection, only 3-chloro-4-fluoroaniline was detected in the batch number 16052301 and R16052501-1 gefitinib samples, but its concentration was below the impurity limit (6 mg/L). This method is simple, reliable, and suitable for the determination of four genotoxic impurities in gefitinib. It can be further applied as a reference for quality control.

15.
Zhongguo Zhong Yao Za Zhi ; 43(18): 3795-3800, 2018 Sep.
Artigo em Chinês | MEDLINE | ID: mdl-30384548

RESUMO

Chinese medicine processing is the main feature that distinguishes traditional Chinese medicine from natural medicine and plant medicine, and is the main feature in clinical medication of traditional Chinese medicine. The research of Chinese medicine processing technology is an important link to realize standardization and standardization of Chinese herbal pieces, with urgent need to attract high attention. At present, there are still many problems in the research of processing technology of Chinese herbal pieces, mainly including inconsistent processing technology, large differences in process technology parameters, and unstable production technology of Chinese herbal pieces, resulting in uncontrollable quality of Chinese herbal pieces and affecting the clinical efficacy of Chinese medicine. This paper focused on the establishment of a unified standard processing technology, and put forward the countermeasures for the processing technology of Chinese medicine based on a comprehensive analysis of the current situations of the processing technology of Chinese herbal pieces, with significance for guiding the establishment of a standardized processing technology of Chinese medicine.


Assuntos
Medicamentos de Ervas Chinesas/química , Medicina Tradicional Chinesa , Tecnologia Farmacêutica/métodos , Controle de Qualidade , Padrões de Referência , Pesquisa
16.
Biomed Chromatogr ; 32(12): e4352, 2018 Dec.
Artigo em Inglês | MEDLINE | ID: mdl-30062682

RESUMO

Xanthii Fructus (XF), a well-known herb in traditional Chinese medicine, has been frequently used for the treatment of allergic rhinitis in the clinic. Its therapeutic metabolic mechanism, however, remains undetermined. In this work, a metabolomics research coupled with metabolic pathway analysis has been employed to screen out the potential mechanism in its effects on allergic rhinitis. Specifically, mouse serum samples containing XF were analyzed based on ultra-high performance liquid chromatography equipped with electrospray ionization quadruple time-of-flight mass spectrometry detection (UHPLC-ESI-Q-TOF-MS) in both positive and negative polarity. In addition, the raw data gained from UHPLC-ESI-Q-TOF-MS were processed by principal component analysis (PCA) and partial least squares discriminant analysis (PLS-DA) in order to discover remarkable metabolites. Twenty-seven potential biomarkers in mouse serum were filtered from free databases like HMDB. Interestingly, this study filtered the potential metabolic pathways including glycerophospholipid metabolism and branch-chain amino acid metabolism. We hope that this paper will provide a feasible strategy for revealing the therapeutic mechanism of XF in allergic rhinitis mice model.


Assuntos
Culinária/métodos , Medicamentos de Ervas Chinesas/farmacologia , Metaboloma/efeitos dos fármacos , Metabolômica/métodos , Aminoácidos de Cadeia Ramificada/metabolismo , Animais , Biomarcadores/sangue , Modelos Animais de Doenças , Glicerofosfolipídeos/metabolismo , Masculino , Camundongos , Camundongos Endogâmicos BALB C , Rinite Alérgica/sangue , Espectrometria de Massas por Ionização por Electrospray
17.
J Sep Sci ; 40(24): 4718-4729, 2017 Dec.
Artigo em Inglês | MEDLINE | ID: mdl-29068518

RESUMO

In China, Semen Cassiae is used clinically to improve eyesight, relieve constipation, and to treat headache and dizziness. Prepared Semen Cassiae is obtained by stir-frying raw Semen Cassiae until it turned dark brown, micro dilatancy, and overflow aroma. After processing, the therapeutic effects change-the purgation effect is alleviated and the hepatoprotective effect is enhanced. To explore the changes in chemical compositions of Semen Cassiae after processing and clarify the material basis of the changed therapeutic effects, an ultra-high performance liquid chromatography with quadrupole time-of-flight mass spectrometry coupled with automated data analysis software and statistical strategy was developed. As a result, 53 compounds in raw Semen Cassiae and 43 compounds in prepared Semen Cassiae were found, a total of 55 chemical compounds were identified. Principle component analysis and t-test were processed by Markerview 1.2.1 software. Finally, 39 peaks were found to be the main contributors to the significant difference (p < 0.05) between raw and prepared Semen Cassiae. Compared with raw Semen Cassiae, 19 peaks showed a higher intensity in prepared Semen Cassiae, while the contents of 20 compounds in prepared Semen Cassiae were lower, most of which belonged to naphthopyrones glycosides and anthraquinone glycosides.


Assuntos
Antraquinonas/isolamento & purificação , Cassia/química , Medicamentos de Ervas Chinesas/química , Glicosídeos/isolamento & purificação , Sementes/química , Cromatografia Líquida de Alta Pressão , Espectrometria de Massas
18.
Acta Pharm Sin B ; 7(2): 185-192, 2017 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-28303225

RESUMO

Cimicifugae Rhizoma (Sheng ma) is a Ranunculaceae herb belonging to a composite family and well known in China. has been widely used in traditional Chinese medicine. The Pharmacopoeia of the People׳s Republic of China contains three varieties (Cimicifuga dahurica (Turcz.), Cimicifuga foetida L. and Cimicifuga heracleifolia Kom.) which have been used clinically as "Sheng-ma". However, the chemical constituents of three components of "Sheng-ma" have never been documented. In this study, a rapid method for the analysis of the main components of "Sheng-ma" was developed using ultra-high performance liquid chromatography with quadrupole-time-of-flight mass spectrometry (UPLC/Q-TOF-MS). The present study reveals the major common and distinct chemical constituents of C. dahurica, C. foetida and C. heracleifolia and also reports principal component and statistical analyses of these results. The components were identified by comparing the retention time, accurate mass, mass spectrometric fragmentation characteristic ions and matching empirical molecular formula with that of the published compounds. A total of 32 common components and 8 markers for different "Sheng-ma" components were identified. These findings provide an important basis for the further study and clinical utilities of the three "Sheng-ma" varieties.

19.
J Pharm Biomed Anal ; 129: 514-534, 2016 Sep 10.
Artigo em Inglês | MEDLINE | ID: mdl-27497653

RESUMO

The approach to investigate traditional Chinese medicine (TCM) is still in its infancy and has been facing enormous challenge. In this paper, a generally applicable strategy was developed for investigation on TCM systematically with an introduced interesting idea about a novel research system which called subchemome. A representative herb-pair, Astragali Radix-Fructus Corni, was successfully employed to expound this novel strategy. Firstly, subchemomes were prepared individually by applying the suitable column chromatography, each of them was detected by UV spectrophotometer or HPLC-DAD detector. The components in each part were then identified based on the mass spectrometric fragmentation patterns and tandem mass spectrometric data by using UHPLC-Q-TOF-MS. Using renal mesangial cell (RMC) viability assay as the evaluation of the pharmacological activity of each group, we developed the new mini herbal formulae aimed at diabetic nephropathy and identified fifteen marker components between the group of new mini herbal formulae and other groups from the angle of the constituent, and then explored the effects of new mini herbal formulae from another angle of the molecular mechanism. Overall, the presently developed strategy should be beneficial and widely used in the investigation on TCM from a new perspective.


Assuntos
Asteraceae/química , Astrágalo (Planta)/química , Cornus/química , Animais , Linhagem Celular , Química Farmacêutica/métodos , Cromatografia Líquida de Alta Pressão/métodos , Medicamentos de Ervas Chinesas/química , Medicina Tradicional Chinesa/métodos , Plantas Medicinais/química , Ratos , Espectrometria de Massas por Ionização por Electrospray/métodos
20.
Mol Cell Endocrinol ; 434: 219-37, 2016 10 15.
Artigo em Inglês | MEDLINE | ID: mdl-27392498

RESUMO

To date, in the struggle against diseases and the development of TCM, what we lack is wisdom rather than knowledge. Studies on pharmacology of traditional Chinese medicine are facing critical challenges on how to select the proper parameters or targets to represent the pharmacological evaluation system. With seven steps of optimized modules established by ourselves, we can re-evaluate TCM in a panorama view with a proper pharmacological evaluation system. In this article, with the treatment of TCM as 'interaction of system to system', a novel and generally applicable approach called fuzzy target contribution recognition was established and agents from Astragali Radix-Fructus Corni in resisting diabetic nephropathy were successfully discovered for the first time. CG6, a promising agent from this herb-pair on the treatment of diabetic nephropathy, was finally acquired and its possible molecular mechanism was explored through a nuclear factor erythroid 2-Like 2 (NFE2L2) activation-dependent pathway.


Assuntos
Cornus/química , Nefropatias Diabéticas/tratamento farmacológico , Medicamentos de Ervas Chinesas/administração & dosagem , Animais , Nefropatias Diabéticas/metabolismo , Medicamentos de Ervas Chinesas/farmacologia , Humanos , Masculino , Medicina Tradicional Chinesa , Camundongos , Fator 2 Relacionado a NF-E2/metabolismo , Ratos , Transdução de Sinais/efeitos dos fármacos , Resultado do Tratamento
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