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1.
Food Chem ; 304: 125397, 2020 Jan 30.
Artigo em Inglês | MEDLINE | ID: mdl-31479996

RESUMO

Branched polyethyleneimine functionalized reduced graphene oxide (BPEIGn) was prepared by a one-step reaction, catalyzed by NaOH, using branched polyethyleneimine (BPEI) and graphene oxide (GO) without reductant hydrazine hydrate or sodium borohydride. The branched polyethylenimine acted as both a grafting agent and a reducing agent of GO. An competitive electrochemical immunosensor based on the Au/sodium mercaptopropanesulfonate/BPEIGn/gold nanoparticles/melamine (Au/MPS/BPEIGn/AuNPs/Mel) modified electrode was constructed for the determination of melamine. The double amplification of BPEIGn and AuNPs increased the sensitivity of the sensor. The melamine was detected by differential pulse voltammetry (DPV) in buffer solution (pH 7.4) containing K3(Fe(CN)6]/K4[Fe(CN)6]. Under optimized conditions, the proposed melamine immunosensor showed a linear relationship in the concentration range of 1 × 10-6 to 1 µM, with a detection limit of 2.66 × 10-7 µM.

2.
Environ Sci Pollut Res Int ; 26(21): 22040-22050, 2019 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-31144181

RESUMO

Exposure to fine particulate matter (PM2.5) could induce lung impairment aggravation. Moreover, endogenous substances are known to play a significant role in lung impairment. Therefore, the research objectives was to investigate the influence of PM2.5-induced lung impairment on the levels of the eight endogenous substances, γ-aminobutyric acid (GABA), acetylcholine (ACh), glutamate (Glu), serotonin (5-HT), 5-hydroxyindole-3-acetic acid (5-HIAA), noradrenaline (NE), dopamine (DA), and 3, 4-dihydroxyphenylacetic acid (DOPAC). A sensitive UPLC-MS/MS method for the simultaneous determination of these endogenous substances in rat plasma and lung tissues was developed. The validated method was successfully applied for comparing profiles of analytes in rat plasma and lung tissues. The results indicated that five endogenous substances, namely, GABA, Ach, Glu, DA, and DOPAC, had a significant change in the rats with PM2.5-induced lung impairment.


Assuntos
Pulmão/metabolismo , Material Particulado/toxicidade , Animais , Cromatografia Líquida , Dopamina , Ácido Glutâmico , Masculino , Neurotransmissores , Ratos , Serotonina , Espectrometria de Massas em Tandem/métodos , Ácido gama-Aminobutírico
3.
Nat Prod Res ; : 1-6, 2018 Oct 30.
Artigo em Inglês | MEDLINE | ID: mdl-30375249

RESUMO

Semen Cuscutae, which mainly consisted of flavonoids, is a traditional Chinese herbal medicine and used for nourishing the liver and kidneys. The aim of this study was to develop a sensitive and selective UPLC-MS/MS method for simultaneous separation and determination of six main active renoprotective components of Hyperoside, Astragalin, Isoquercitrin, Quercitrin, Quercetin, and Kaempferol from Semen Cuscutae in rat plasma, and to reveal the pharmacokinetic differences between normal and kidney deficient rats. The validated method has been successfully applied to comparing pharmacokinetic profiles of the six analytes in rat plasma. The results indicated that there was significant difference in pharmacokinetic parameters of the six analytes between two groups, while absorptions in kidney deficient group were significantly lower than those in normal group. This study would be helpful for evaluating the Semen Cuscutae as renoprotective drug candidates for pre-clinical and clinical research.

4.
J Chromatogr B Analyt Technol Biomed Life Sci ; 1061-1062: 176-184, 2017 Sep 01.
Artigo em Inglês | MEDLINE | ID: mdl-28738255

RESUMO

Viscum coloratum is a perennial evergreen, semi-parasitic plant. It is generally used for treating cardiovascular diseases, cancer, hepatitis and hemorrhage. In this study, reliable methods were developed for the qualitative and quantitative analysis of the common constituents in Viscum coloratum and its corresponding host. In the rapid qualitative analysis, a method of ultra-high performance liquid chromatography and quadrupole time-of-flight tandem mass spectrometry was established for identification of the same compounds. Based on the retention times, accurate mass measurement and previous literatures, 23 components were clearly identified by comparison with reference substances. In the quantitative analysis, a method for Viscum coloratum and its corresponding host was developed by ultra-high performance liquid chromatography with triple quadrupole mass spectrometry. 13 common compounds of viscum coloratum and host plants from 19 batches were analyzed with a good linearity (r2≥0.9991), intra-day precision (RSD≤3.24%), inter-day precision (RSD≤3.31%), repeatability (RSD≤2.43%), stability (RSD≤2.63%), and recovery (98.2-102.4%). The overall limits of quantification were less than 5.0ng/mL. The results indicated that these effective and comprehensive methods can be applicable to simultaneous qualitative and quantitative analysis of these common compounds presented in Viscum coloratum and corresponding host plants.


Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Flavonoides/análise , Extratos Vegetais/química , Espectrometria de Massas em Tandem/métodos , Viscum/química , Flavonoides/química , Flavonoides/isolamento & purificação , Limite de Detecção , Modelos Lineares , Reprodutibilidade dos Testes
5.
Mater Sci Eng C Mater Biol Appl ; 68: 308-316, 2016 Nov 01.
Artigo em Inglês | MEDLINE | ID: mdl-27524025

RESUMO

The triethylenetetramine-functionalized graphene (TFGn) was prepared using graphene oxide (GO) and triethylenetetramine as raw materials through a one-step reaction under alkaline condition. The triethylenetetramine not only acted as cross-linker to combine GO, but also as reductant of GO. The TFGn was characterized by its ultraviolet spectrum (UV), Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), Raman spectroscopy and Scanning electron microscopy (SEM). The results showed that triethylenetetramine was successfully grafted onto the surface of the GO through covalent bonding between amine and epoxy groups. The resultant TFGn was uniformly dispersed in water over several weeks, suggesting that the introduction of amino groups greatly increased the hydrophilicity of TFGn. The triethylenetetramine-functionalized graphene was then applied to fabricate glucose biosensors with IO4(-) oxidized glucose oxidase (GOx) through layer-by-layer (LBL) self-assembly by the covalent bonding between the aldehyde groups of GOx and amino groups of TFGn. The gold electrodes modified with the (GOx/TFGn)n multilayer films were studied by cyclic voltammetry (CV) and showed outstanding electrocatalytical response to the oxidation of glucose when ferrocenemethanol was used as an artificial redox mediator. The response increased with an increasing number of GOx/TFGn bilayers, indicating that the analytical performance, such as the sensitivity of the glucose biosensor, could be adjusted by tuning the number of deposited GOx/TFGn bilayers. The linear response range of the biosensor constructed with six bilayers of GOx/TFGn to the concentration of glucose can extend to at least 8mM with a sensitivity of 19.9µAmM(-1)cm(-2). In addition, the sensor exhibited good stability due to the covalent interactions between the GOx and TFGn.


Assuntos
Técnicas Biossensoriais/métodos , Glucose Oxidase/química , Glucose/análise , Grafite/química , Trientina/química
6.
Pharmacogn Mag ; 11(43): 455-62, 2015 Jul-Sep.
Artigo em Inglês | MEDLINE | ID: mdl-26246719

RESUMO

BACKGROUND: Viscum coloratum (Komar) Nakai, known as Hujisheng in china, has been widely used as a herb medicine to treat a variety of diseases, including cardiovascular diseases, cancer, hypertension, hepatitis and hemorrhage. OBJECTIVE: The aim was to investigate pharmacokinetic interactions among co-existing ingredients in V. coloratum after intravenous administration of three different preparations (four monomer solutions, the mixture of them and Viscum coloratum extracts) to rats. MATERIALS AND METHODS: After protein precipitation pretreatment with plasma samples, high performance liquid chromatographic methods were developed and applied to quantitatively determinate the four components [syringin (Syri), homoeriodictyol-7-O-ß-D-glycoside (Hedt-III), homoeriodictyol-7-O-ß-D-apiose (1 → 2)-ß-D-glycoside (Hedt-II) and homoeriodictyol-7-O-ß-D-apiosiyl-(1 → 5)-ß-D-apiosyl-(1 → 2)-ß-D-glycoside (Hedt-I)]. The pharmacokinetic parameters (Area under the curve [AUC(0-t)], AUC(0-∞), t 1/2) were calculated using DAS 2.1 software (Chinese Pharmacological Society, Shanghai, China) and compared statistically by One-way analysis of variance using SPSS software (18.0, Chicago, IL, USA) with P < 0.05 considered statistically significant. RESULTS: Good linearities were achieved in the measured concentration range with R (2) it0.9920. Precision, accuracy and extraction recovery were all within the acceptable range. For Syri, there was a significant difference only on t 1/2 among three treatment groups. For Hedt-I, Hedt II and Hedt-III, three flavonoid glycosides, the change of AUC(0-t), AUC(0-∞) and t 1/2 were markedly distinctive and even converse. CONCLUSION: Complex, extensive pharmacokinetic interactions were observed among these components in V. coloratum. They were mutually influenced by the in vivo absorption, distribution, metabolism and elimination. The result suggested traditional Chinese medicine was a complicated system, and we should take a scientific and dialectic view in the research and development processes.

7.
J Sep Sci ; 38(3): 530-40, 2015 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-25402838

RESUMO

A simple, specific, and sensitive ultra high performance liquid chromatography with tandem mass spectrometry method was developed and validated for the simultaneous quantification of nine compounds including a new compound, rhamnazin-3-Ο-ß-D-(6″-ß-hydroxy-ß-methyglutaryl)-ß-D-glucoside-4'-Ο-ß-D-glucoside, in rat plasma using baicalin as an internal standard. The plasma samples were pretreated and extracted by protein precipitation with 0.2% formic acid in acetonitrile. The analytes were separated on a Thermo Syncronis C18 column by gradient elution with a mobile phase consisting of acetonitrile and 0.1% aqueous formic acid at a flow rate of 0.25 mL/min. The detection of the analytes was performed on an electrospray ionization interface operating in positive-ion and multiple reaction monitoring acquisition modes. The calibration curves of these analytes showed good linearity (r > 0.99) within the test ranges. The lower limit of quantification ranged from 0.4 to 20.1 ng/mL for the analytes. The intra- and interday precision and accuracy were all within ±15%, and the recoveries were higher than 80.0%. The validated method was successfully applied to a pharmacokinetic study of the nine flavonoids after administration of the Viscum coloratum extracts by intravenous injection.


Assuntos
Flavonoides/sangue , Flavonoides/farmacocinética , Extratos Vegetais/química , Viscum/química , Animais , Cromatografia Líquida de Alta Pressão , Flavonoides/administração & dosagem , Flavonoides/química , Injeções Intravenosas , Masculino , Estrutura Molecular , Extratos Vegetais/administração & dosagem , Extratos Vegetais/sangue , Extratos Vegetais/farmacocinética , Ratos , Ratos Wistar , Espectrometria de Massas em Tandem
8.
Drug Test Anal ; 7(6): 544-9, 2015 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-25209951

RESUMO

TM-2 is a novel semi-synthetic taxane derivative, selected for preclinical development based on its greater anticancer activity and lower toxicity compared with docetaxel. In this study, a rapid and sensitive analytical method based on ultra performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) has been developed for the determination of TM-2 in rat plasma. The biological samples were extracted with methyl tert-butyl ether and separated on a C18 column (50 mm × 2.1 mm, 1.7 µm) using a mobile phase consisting of acetonitrile and 2 mM ammonium acetate. The standard curves were linear over the range 5-1000 ng/mL in rat plasma. The precision (relative standard deviation, RSD, %) were within 14.5%, and the accuracy (relative error, RE, %) ranged from -1.56 to 2.36%. Recovery and matrix effect were satisfactory in rat plasma. The validated method was successfully applied to pharmacokinetic studies after intravenous administration of TM-2 to rats. The pharmacokinetics of TM-2 in rats were characterized by a large volume of distribution and a long half-life of elimination after single dose (4, 8, and 16 mg/kg), and a good correlation was observed between AUC and dose. The preclinical data will be useful for the design of subsequent trials of TM-2.


Assuntos
Antineoplásicos/farmacocinética , Taxoides/farmacocinética , Animais , Antineoplásicos/análise , Antineoplásicos/sangue , Cromatografia Líquida , Relação Dose-Resposta a Droga , Feminino , Masculino , Ratos , Espectrometria de Massas em Tandem , Taxoides/análise , Taxoides/sangue
9.
J Sep Sci ; 37(6): 625-9, 2014 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-24449563

RESUMO

TM-2 (13-(N-Boc-3-i-butylisoserinoyl-4,10-ß-diacetoxy-2-α-benzoyloxy-5-ß-20-epoxy-1,13-α-dihydroxy-9-oxo-19-norcyclopropa[g]tax-11-ene) is a novel semisynthetic taxane derivative. Our previous study suggested that TM-2 is a promising antitumor analogue. In this paper, the metabolism of TM-2 was investigated in rats following intravenous administration. Two different types of mass spectrometry-hybrid linear trap quadrupole orbitrap (LTQ-Orbitrap) mass spectrometry and triple-quadrupole tandem (QQQ) mass spectrometry-were employed to acquire structural information of TM-2 metabolites. A total of 17 components were identified as the metabolites of TM-2 in bile, feces, and urine samples. Accurate mass measurement using LC-LTQ-Orbitrap-MS was used to determine the accurate mass data and elemental composition of metabolites thereby confirming the proposed structures of the metabolites. The metabolites proposed were mainly oxidates of TM-2, including methoxy, hydroxyl, dihydroxy, and trihydroxyl analogues. The major metabolic pathway of TM-2 was the hydroxylation of the taxane ring or the lateral chain. These important metabolic data serve as a useful resource to support further research of TM-2.


Assuntos
Antineoplásicos/análise , Antineoplásicos/metabolismo , Taxoides/química , Taxoides/metabolismo , Administração Intravenosa , Animais , Antineoplásicos/administração & dosagem , Cromatografia Líquida , Feminino , Masculino , Espectrometria de Massas , Conformação Molecular , Ratos , Ratos Sprague-Dawley , Taxoides/administração & dosagem
10.
J Sep Sci ; 37(4): 352-9, 2014 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-24318005

RESUMO

Opioid and ephedra alkaloids known as the active ingredients for Keke capsule, which is used to treat coughs and bronchial asthma, could have potential adverse effects on the central nervous system. Therefore, an efficient, sensitive rapid-resolution LC-MS/MS method for the simultaneous determination of morphine, ephedrine, and pseudoephedrine in rat plasma and brain tissue homogenate has been developed. The method was validated in the plasma and brain tissue samples, showed good linearity over a wide concentration range (r(2) > 0.99). The intra- and interday assay variability was less than 15% for all analytes, and the accuracy was between -8.8 and 5.7%. The study provided the pharmacokinetics profiles and the brain regional distribution of the three active alkaloids after oral administration of Keke capsule. The results also indicated that significant difference in pharmacokinetics parameters of the epimers was observed between ephedrine and pseudoephedrine.


Assuntos
Efedrina/farmacocinética , Morfina/farmacocinética , Administração Oral , Animais , Encéfalo , Cromatografia Líquida de Alta Pressão , Efedrina/administração & dosagem , Efedrina/química , Masculino , Conformação Molecular , Morfina/administração & dosagem , Morfina/química , Ratos , Ratos Wistar , Estereoisomerismo , Espectrometria de Massas em Tandem , Distribuição Tecidual
11.
J Pharm Biomed Anal ; 88: 416-22, 2014 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-24176746

RESUMO

Schisandra chinensis (Turcz.) Baill. has been used as a sedative and hypnotic agent in traditional Chinese medicine for centuries. The purpose of this study was to reveal the influence of insomnia on the levels of the neurotransmitters: glutamate (Glu), γ-aminobutyric acid (GABA), noradrenaline (NE), dopamine (DA), serotonin (5-HT) and their metabolites (5-HIAA, DOPAC and HVA), and to study the role of S. chinensis in the treatment of insomnia. To achieve this goal, an efficient, sensitive and selective method was developed and validated for the simultaneous determination of these five neurotransmitters and their metabolites in rat brain samples using ultra fast liquid chromatography/tandem mass spectrometry (UFLC-MS/MS). The analysis was performed on a Synergi Fusion-RP 80A ODS column (150mm×2.0mm, 4.0µm) using gradient elution, with the mobile phase consisting of acetonitrile and 0.05% formic acid in water. The method was validated using rat brain homogenate samples and showed a good linearity over a wide concentration range (r(2)>0.99) with a lower limit of quantification (LLOQ) at 4-16ngmL(-1). The intra and inter-day assay variability was less than 15% for all analytes. The results indicated that the condition of insomnia elevated GABA, NE, DA, DOPAC and HVA, and reduced 5-HT, 5-HIAA levels in rat brain. The oral administration of S. chinensis (7.5gkg(-1)day(-1), eight days) influenced insomnia by significantly increasing or reducing the levels of the neurotransmitters parameters mentioned above. These results suggested that S. chinensis could alter the levels of these brain neurotransmitters and their metabolites through its sedative-hypnotic effects.


Assuntos
Aminas/análise , Aminoácidos/análise , Encéfalo/efeitos dos fármacos , Neurotransmissores/análise , Animais , Encéfalo/metabolismo , Cromatografia Líquida de Alta Pressão , Hipnóticos e Sedativos/análise , Masculino , Medicina Tradicional Chinesa , Controle de Qualidade , Ratos , Ratos Sprague-Dawley , Reprodutibilidade dos Testes , Schisandra/metabolismo , Espectrometria de Massas em Tandem
12.
J Mass Spectrom ; 48(4): 448-58, 2013 Apr.
Artigo em Inglês | MEDLINE | ID: mdl-23584938

RESUMO

Schisandra chinensis (Turcz.) Baill., a traditional Chinese medicine, has been clinically used for the treatment of insomnia for centuries. The insomnia mechanism and the possible active ingredients of S. chinensis remain largely unknown. The objective of this study was to develop a method to detect its components which could pass through the blood brain barrier (BBB) by determining the brain microdialysate and brain tissue homogenate samples and then obtain the pharmacokinetic profile in brain for comprehensive understanding of its hypnotic clinical efficacy. Therefore, an efficient, sensitive and selective ultra fast liquid chromatography/tandem mass spectrometry method for the simultaneous determination of six sedative and hypnotic lignans (schisandrin, schisandrol B, schisantherin A, deoxyshisandrin, γ-schisandrin and gomisin N) of Schisandra chinensis (Turcz.) Baill. in rat brain tissue homogenate and brain microdialysates has been developed and validated. The analysis was performed on a Shim-pack XR-ODS column (75 mm × 3.0 mm, 2.2 µm) using gradient elution with the mobile phase consisting of acetonitrile and 0.1% formic acid water. The method was validated in brain homogenate and microdialysate samples, which all showed good linearity over a wide concentration range (r(2)> 0.99), and the obtained lower limit of quantification was 0.1 ng · ml(-1) for the analytes in brain microdialysate samples. The intra- and inter-day assay variability was less than 15% for all analytes. The study proved the six lignans, as sedative and hypnotic ingredients, could pass through the BBB with brain targeting, distributed mainly in the hypothalamus and possessed complete pharmacokinetics process in brain. The results also indicated that significant difference in pharmacokinetic parameters of the analytes was observed between two groups, while absorptions of these analytes in insomniac group were significantly better than those in normal group.


Assuntos
Química Encefálica , Medicamentos de Ervas Chinesas/química , Lignanas/análise , Schisandra/química , Distúrbios do Início e da Manutenção do Sono/metabolismo , Animais , Área Sob a Curva , Cromatografia Líquida de Alta Pressão/métodos , Estabilidade de Medicamentos , Medicamentos de Ervas Chinesas/administração & dosagem , Medicamentos de Ervas Chinesas/farmacocinética , Medicamentos de Ervas Chinesas/farmacologia , Hipnóticos e Sedativos , Lignanas/química , Lignanas/farmacocinética , Modelos Lineares , Masculino , Microdiálise , Ratos , Ratos Sprague-Dawley , Reprodutibilidade dos Testes , Sensibilidade e Especificidade , Espectrometria de Massas em Tandem/métodos
13.
J Pharm Biomed Anal ; 77: 120-7, 2013 Apr 15.
Artigo em Inglês | MEDLINE | ID: mdl-23416367

RESUMO

Schisandra chinensis (Turcz.) Baill., a traditional Chinese medicine, has been used for treating insomnia for centuries. This paper was designed to study on the plasma pharmacokinetic for its absorption process, and to compare the pharmacokinetics of its active ingredients in normal and insomnic rats orally administrated with the prescription. Therefore, an efficient, sensitive and selective ultra fast liquid chromatography/tandem mass spectrometry (UFLC-MS/MS) method for the simultaneous determination of six sedative and hypnotic lignans (schisandrin, schisandrol B, schisantherin A, deoxyshisandrin, γ-schisandrin and gomisin N) of Schisandra chinensis (Turcz.) Baill. in rat plasma has been developed and validated. The analysis was performed on a Shim-pack XR-ODS column (75mm×3.0mm, 2.2µm) using gradient elution with the mobile phase consisting of acetonitrile and 0.1% formic acid waterat a flow rate of 0.4ml/min. The detection of the analytes was performed on 4000Q UFLC-MS/MS system with turbo ion spray source in the positive ion and multiple reaction-monitoring mode. The method was validated in plasma samples, which showed good linearity over a wide concentration range (r(2)>0.99), and obtained lower limits of quantification were 10, 1.2, 1.2, 1.2, 1.0 and 1.2ngmL(-1) for the analytes. The intra- and inter-day assay variability was less than 15% for all analytes. The mean extraction recoveries of analytes and IS from rats plasma were all more than 85.0%. The validated method has been successfully applied to comparing pharmacokinetic profiles of analytes in rat plasma. The results indicated that significant difference in pharmacokinetic parameters of the analytes was observed between two groups, while absorptions of these analytes in insomnic group were all significantly higher than those in normal group.


Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Lignanas/sangue , Lignanas/farmacocinética , Schisandra/química , Espectrometria de Massas em Tandem/métodos , Animais , Ciclo-Octanos/sangue , Ciclo-Octanos/química , Ciclo-Octanos/farmacocinética , Dioxóis/sangue , Dioxóis/química , Dioxóis/farmacocinética , Medicamentos de Ervas Chinesas/química , Medicamentos de Ervas Chinesas/farmacocinética , Lignanas/química , Masculino , Medicina Tradicional Chinesa , Compostos Policíclicos/sangue , Compostos Policíclicos/química , Compostos Policíclicos/farmacocinética , Distribuição Aleatória , Ratos , Ratos Sprague-Dawley , Sensibilidade e Especificidade , Distúrbios do Início e da Manutenção do Sono/tratamento farmacológico
14.
World J Hepatol ; 4(12): 389-93, 2012 Dec 27.
Artigo em Inglês | MEDLINE | ID: mdl-23355917

RESUMO

AIM: To study the effect of rescue monotherapy with adefovir (ADV) in patients with chronic hepatitis B (CHB) who developed drug resistance to lamivudine (LAM). METHODS: A total of 76 treated CHB patients with resistance to LAM were enrolled in the present study. The patients' baseline characteristics, such as age, gender, blood tests and hepatitis B virus (HBV) DNA were collected; therapy duration and the response of each patient were also recorded. ADV monotherapy was set as the observation group A. Twenty-four patients with LAM resistance, who were set as group B, accepted combined therapy with LAM + ADV. Patients were followed up at 0, 12, 24, 52, 104 and 156 wk. Hepatitis B surface antigen status, hepatitis B e antigen (HBeAg)/anti-HBe status, HBV DNA level and biochemical indexes were monitored. Sequencer of HBV polymerase gene was performed on the ABI 3730 automated sequencer. If no desired effects had been achieved during the course of treatment, patients' choices were also taken into account. The control group was tested at the same time. RESULTS: In the two groups, 27 cases developed viral breakthrough after LAM treatment response. The remaining 49 cases underwent biochemical rebound accompanied by rtM204I/V or rtL180M mutation. In group A, 52 cases finished 156 wk of ADV monotherapy; of whom, 36 cases were HBeAg positive and 16 HBeAg negative. In patients whose baseline HBV DNAs were 10(3)-10(5) copies/mL, 88.8% of patients' HBV DNAs were lower than the lower test limit (10(3) copies/mL) after 12 to 156 wk of ADV treatment. In patients whose baseline HBV DNAs were ≥ 10(6) copies/mL, 41.1%-47.0% of patients' HBV DNAs were lower than the lower test limit after the same course of ADV therapy (χ(2) were 4.35-5.4, 41.1%-47.0% vs 88.8% group 10(3)-10(5) copies/mL, P < 0.01). In group A, seroconversion of HBeAg developed in 8 of 36 cases (22.2%). In group B, 24 cases finished 156 wk of LAM + ADV; of whom, 17 cases were HBeAg positive and 7 HBeAg negative. In patients whose baseline HBV DNAs were 10(3)-10(5) copies /mL, 81.8% of patients' HBV DNAs were lower than the lower test limit (10(3) copies/mL) after 12 to 156 wk of treatment. In the patients whose baseline HBV DNAs were ≥ 10(6) copies/mL, 46.1%-53.8% of patients' HBV DNAs were lower than the lower test limit after the same course of LAM + ADV therapy (χ(2) were 4.1-5.0, 46.1%-53.8% vs 81.8% group 10(3)-10(5) copies/mL, P < 0.05-0.01). In group B, 4 of 17 cases (23.5%) developed seroconversion of HBeAg. Treatment outcomes in groups A and B were comparable. CONCLUSION: In both group A and B, the ratios of virological response have similar efficacy in patients with lower baseline HBV DNAs.

15.
Chem Pharm Bull (Tokyo) ; 59(11): 1322-8, 2011.
Artigo em Inglês | MEDLINE | ID: mdl-22041066

RESUMO

A high-performance liquid chromatographic-mass spectrometric method was developed for the simultaneous determination of 10 flavonoids in Viscum coloratum obtained from different host species and different sources. Viscum coloratum was extracted with 50% methanol. The extracts were separated on a C(18) column with a gradient of 0.1% (v/v) formic acid and methanol. The flavonoids in the extracts were detected by negative electrospray ionization mass spectrometry in selective ion monitoring mode. The calibration curves showed good linearity (r>0.998) within the test ranges (homoeriodictyol: 0.149-8.940 µg/ml, homoeriodictyol-7-O-ß-D-glycoside: 0.230-13.80 µg/ml, homoeriodictyol-7-O-ß-D-apiose (1→2)-ß-D-glycoside: 5.000-300.0 µg/ml, homoeriodictyol-7-O-ß-D-apiose (1→5)-ß-D-apiose (1→2)-ß-D-glycoside: 0.835-125.3 µg/ml, rhamnazin-3-O-ß-D-glucoside: 0.064-3.840 µg/ml, rhamnazin-3-O-ß-D-(6″-ß-hydroxy-ß-methyglutaryl)-glucoside: 1.435-86.10 µg/ml, isorhamnetin-3-O-ß-D-glucoside: 0.930-55.80 µg/ml, 5-hydroxy-3,7,3'-trimethoxyflavone-4'-O-ß-D-glucoside: 0.067-4.020 µg/ml, 5,7,4'-trihydroxy-3,3'-dimethoxyflavone: 0.270-16.20 µg/ml, pachypodol: 0.110-6.600 µg/ml). The limits of quantification were between 0.006-0.720 µg/ml. The assay was reproducible and the overall intra- and inter-day variations were less than 4.6%. The recoveries varied from 93.4 to 103.9% at three different concentration levels. The validation method was used to determine the contents of 10 flavonoids in Viscum coloratum. A one-way analysis of variance was applied to evaluate Viscum coloratum-host-source interactions. Compared with the host species, the sample source had a significant impact on the sample content.


Assuntos
Flavonoides/química , Viscum/química , Calibragem , Cromatografia Líquida de Alta Pressão/normas , Flavonoides/isolamento & purificação , Espectrometria de Massas por Ionização por Electrospray/normas
16.
J Pharm Anal ; 1(2): 113-118, 2011 May.
Artigo em Inglês | MEDLINE | ID: mdl-29403689

RESUMO

A high-Performance liquid chromatography coupled ultraviolet (HPLC-UV) method was developed for a chemical fingerprint analysis of Viscum coloratum. Eighteen peaks were selected as the common peaks and Homoeriodictyol-7-0-ß-D-apiosiyl-(1→2)-ß-D-glucoside was used as a reference. The relative areas of common peaks were used for hierarchical clustering analysis and similarity calculation. Thirty-seven samples collected from different sources were classified into five groups. The similarities of 21 batches Viscum coloratum samples were beyond 0.90. The results obtained suggest that the Chromatographie fingerprint can efficiently identify Viscum coloratum. Additionally, the fingerprints can then be used to evaluate the correlation between Viscum coloratum and hosts.

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