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1.
Zhongguo Zhong Yao Za Zhi ; 44(10): 2139-2148, 2019 May.
Artigo em Chinês | MEDLINE | ID: mdl-31355573

RESUMO

In this paper,ultra performance liquid chromatography coupled with time-of-flight mass spectrometry( UPLC-Q-TOFMS) technique was used to study the effects of steamed notoginseng on endogenous markers in plasma of rats with hemolytic anemia induced by N-acetyl phenyl hydrazine( APH). The aim was to find out the potential biomarkers and possible blood enriching mechanism of steamed notoginseng on hemolytic anemia rats. In the experiment,steamed notoginseng medicine pair( steamed notoginseng-ginseng)and compound medicines( Sanqi Yangxue Capsules) were used respectively to intervene in APH-induced hemolytic anemia model rats.Then blood routine indexes such as red blood cells( RBC),hemoglobin( Hb) and related organ indexes were determined. As compared with the blank group,the RBC and Hb levels in the model group were substantially decreased( P< 0. 01),while the liver and spleen organ indexes were increased( P< 0. 05). The results of blood routine and organ index demonstrated that the blood deficiency model was successfully established. Steamed notoginseng can significantly increase the RBC level of rats( P<0. 01),and the related indicators of each drug group had a trend of returning to normal levels,verifying the blood enriching effect of steamed notoginseng. The UPLC-Q-TOF-MS technique,principal component analysis( PCA) and partial least squares-discrimination analysis( PLS-DA) were used to analyze the metabolic profiles between the normal group and the model group. Twenty-six potential biomarkers for hemolytic anemia were screened in plasma. Nine metabolites such as retinol,L-valine,and arachidonic acid were down-regulated in the blood deficiency rats,and 17 metabolites such as protoporphyrin Ⅸ and niacinamide were up-regulated. The metabolic level of biomarkers could be changed to a normal state after rats were given with steamed notoginseng,drug pairs,and compound prescriptions. It can be speculated that steamed notoginseng may play a role of blood tonifying by improving biosynthesis of valine,leucine and isoleucine,as well as metabolic pathways such as retinol metabolism and arachidonic acid metabolism.


Assuntos
Anemia Hemolítica/tratamento farmacológico , Medicamentos de Ervas Chinesas/farmacologia , Metabolômica , Panax notoginseng/química , Animais , Biomarcadores , Espectrometria de Massas , Metaboloma , Ratos , Vapor
2.
J Chromatogr A ; 1601: 335-339, 2019 Sep 13.
Artigo em Inglês | MEDLINE | ID: mdl-31155143

RESUMO

Sodium valproate is the most commonly used antiepileptic drug that patients need to keep taking over a long period of time or on a permanent basis. Its blood concentration should be accurately detected to avoid toxicity or side-effects, especially for children and the aged. Dried blood spot (DBS) sampling from finger prick is a minimally invasive and patient-friendly procedure for blood collection. However, there are few studies about rapid detection of sodium valproate in DBS samples in current literatures. In this work, we developed an ink auxiliary headspace gas chromatography mass spectrometry (GC-MS) strategy for direct detection of sodium valproate in DBS from epilepsy patients, which does not need extra solvent extraction or elution. It was discovered that carbon black ink could provide better capacity of heat absorption and dissociation, and higher quality of headspace sampling. The detection sensitivity has been improved with reported headspace GC-MS methods, and the limit of quantitation could reach to 200 ng/mL. Finally, this strategy was practically applied to quantify sodium valproate in DBS samples from 29 epilepsy patients. The result showed higher accuracy with lower relative errors by comparing with the clinical immunoassay results. In conclusion, we developed a direct detection method for DBS samples that is suitable for high-throughput clinical test with great potential for clinical application.


Assuntos
Teste em Amostras de Sangue Seco/métodos , Cromatografia Gasosa-Espectrometria de Massas , Ácido Valproico/análise , Anticonvulsivantes/análise , Anticonvulsivantes/sangue , Criança , Monitoramento de Medicamentos , Humanos , Manejo de Espécimes , Ácido Valproico/sangue
3.
J Pharm Biomed Anal ; 174: 367-375, 2019 Sep 10.
Artigo em Inglês | MEDLINE | ID: mdl-31202879

RESUMO

Fufang Danshen Dripping Pill (FDDP) and Clopidogrel Bisulfate Tablet (CBT) are usually combined for treatment of coronary artery diseases in clinical. To investigate the pharmacokinetic interaction between FDDP and CBT after oral administration of FDDP, CBT and their combination in rats, a novel LC-MS method with segmented scan modes (multiple reaction monitoring and selected ion monitoring) and polarity (positive and negative ionization) was developed. Clopidogrel and the main active ingredients of FDDP, with different chemical and ionization properties, were simultaneously quantified in plasma in a single run. The method was validated in terms of specificity, linearity, precision, accuracy, recovery, matrix effect and stability. As a result, co-administration of FDDP and CBT significantly altered the pharmacokinetic parameters of danshensu, ginsenoside Rb1, dihydrotanshinone I, tanshinone I and tanshinone IIA of FDDP, as well as clopidogrel. Mechanism studies suggested that induction of liver cytochrome P450 isozymes CYP2C11 and CYP3A1 by co-administration, as well as inhibition of carboxyl esterase 1, was partly responsible for FDDP-CBT pharmacokinetic interactions. The developed LC-MS method could be used to simultaneously quantify different types of in vivo analytes in a single run, and the results could be used for clinical medication guidance of FDDP and CBT.

4.
Phytomedicine ; 58: 152866, 2019 May.
Artigo em Inglês | MEDLINE | ID: mdl-30831464

RESUMO

BACKGROUND: Herbal compatibility of compound formulas can enhance therapeutic effects or reduce side effects of the monarch drugs, but majority of compatibility mechanisms are still unknown. Sangju-Yin, a well-known Chinese compound formula, is currently used to treat common cold in clinical. PURPOSE: In this study, we proposed a strategy to explore the compatibility mechanism of Sangju-Yin by investigating P450 enzymes-based metabolic interactions between monarch drugs and the other constituent herbs. METHODS: Under the guidance of traditional Chinese medicine theory, the constituent herbs of Sangju-Yin were divided into four groups, including monarch drugs, monarch drugs with addition of minister drugs, monarch drugs with addition of minister and adjuvant drugs, as well as the whole recipe, namely monarch drugs with addition of minister, adjuvant and conductant drugs. Their effects on rats in vivo P450 (CYP1A2, CYP2A3, CYP2C6, CYP2C11 and CYP3A1) activities after oral administration were evaluated using probe drug assay based on LC-MS/MS. Moreover, effects of the four groups of herbs on mRNA expression of P450 enzymes after oral administration, as well as in vitro P450 activities after co-incubation, were investigated to explore the underlying mechanisms. RESULTS: Comparing with monarch drugs, addition of different constituent herbs significantly enhanced CYP1A2 and CYP2C6 activities, and inhibited CYP2A3 and CYP3A1 activities, indicating their possible influences on plasma concentrations of active constituents in the monarch drugs. Mechanism study suggested that these herbs affected P450 activities by transcriptional regulation and/or direct interaction with the enzymes. CONCLUSION: This study clarified the compatibility mechanism of Sangju-Yin from the aspect of P450 enzymes-based metabolic interactions, which would benefit better understanding of the therapeutic basis of Sangju-Yin.


Assuntos
Sistema Enzimático do Citocromo P-450/efeitos dos fármacos , Composição de Medicamentos , Interações de Medicamentos , Medicamentos de Ervas Chinesas/administração & dosagem , Medicina Tradicional Chinesa , Animais , Cromatografia Líquida , Sistema Enzimático do Citocromo P-450/metabolismo , Medicamentos de Ervas Chinesas/química , Masculino , Distribuição Aleatória , Ratos , Ratos Sprague-Dawley , Espectrometria de Massas em Tandem
5.
J Ethnopharmacol ; 234: 189-196, 2019 Apr 24.
Artigo em Inglês | MEDLINE | ID: mdl-30703494

RESUMO

ETHNOPHARMACOLOGICAL RELEVANCE: Clopidogrel is the recommended treatment by current clinical practice guidelines to prevent adverse cardiovascular events in patients with coronary heart disease (CHD), but this treatment regimen still fails and 5-40% patients display inadequate antiplatelet responses. Fufang Danshen Dripping Pill (FDDP), a Chinese patient drug, was used as the combination with clopidogrel to improve the therapeutic effect. However, the mechanism of the interaction between clopidogrel and FDDP has not been elucidated. MATERIALS AND METHODS: We have used non-targeted metabolism method based on GC-MS and LC-MS for the investigation of drug interactions between clopidogrel and FDDP. 63 patients were divided into four groups with different dosage regimen and the serum samples were collected for the analysis. RESULTS: We have found 5 and 55 differential metabolites between health volunteer group and CHD patients group, respectively. The contents of these differential metabolites had diverse changes in clopidogrel group, FDDP group, and drug combination group, indicating that the clopidogrel and FDDP combination can adjust the glycometabolism, lipid metabolism, and phospholipid metabolism, sequentially made the content of downstream related metabolites towards to the health volunteer group. CONCLUSION: This work has explained the mechanism of the interaction between clopidogrel and FDDP from the point of view of metabolic product change, and revealed the potential metabolic pathways it affects, which provided the new ideas for clinical medication.


Assuntos
Clopidogrel/administração & dosagem , Doença das Coronárias/tratamento farmacológico , Medicamentos de Ervas Chinesas/administração & dosagem , Adolescente , Adulto , Idoso , Idoso de 80 Anos ou mais , Estudos de Casos e Controles , Cromatografia Líquida , Clopidogrel/farmacologia , Doença das Coronárias/metabolismo , Relação Dose-Resposta a Droga , Medicamentos de Ervas Chinesas/farmacologia , Cromatografia Gasosa-Espectrometria de Massas , Interações Ervas-Drogas , Humanos , Metabolismo dos Lipídeos/efeitos dos fármacos , Espectrometria de Massas , Metabolômica/métodos , Pessoa de Meia-Idade , Inibidores da Agregação de Plaquetas/administração & dosagem , Inibidores da Agregação de Plaquetas/farmacologia , Adulto Jovem
6.
Artigo em Inglês | MEDLINE | ID: mdl-30690396

RESUMO

Ginkgo biloba leaves extract (GBE), one of the most widely used traditional Chinese medicines worldwide, can be used for the treatment of diabetes mellitus (DM). However, its biotransformation in liver is not fully known under the state of DM. In this study, an off-line hydrophilic interaction × reversed-phase two-dimensional liquid chromatography (HILIC × RP 2D-LC) system coupled with diode array detection (DAD) and quadrupole time-of-flight mass spectrometry (q/TOF-MS) was established for the qualification and quantification of the biotransformation of GBE in normal and diabetic rat liver microsomes (RLMs). 6 metabolites were tentatively identified according to the exact molecular weights and the characteristic fragment ions provided by q/TOF-MS data. The results of metabolic stability showed that the metabolic ratio of four target compounds including quercetin, genistein, kaempferol and isorhamnetin in diabetic RLMs were significantly enhanced when comparing with normal RLMs. The results of enzyme kinetics showed that compared with normal RLMs, the Michaelis-Menten constant (Km) value of genistein was obvious increased while its maximal velocity (Vmax) and intrinsic clearance (CLint) values were significantly decreased by diabetic RLMs, and the Vmax and CLint values of kaempferol and isorhamnetin were notably enhanced while their Km values were markedly reduced. For the half-time (t1/2) values of four target compounds and the Km, Vmax and CLint values of quercetin, there were not statistically significant changes between normal and diabetic RLMs. The results suggest that the developed off-line 2D LC-DAD-q/TOF-MS method is an easy and accurate approach for the study of GBE biotransformation in RLMs and may provide the essential data for further pharmacological and clinical studies of GBE.


Assuntos
Cromatografia de Fase Reversa/métodos , Espectrometria de Massas/métodos , Microssomos Hepáticos/metabolismo , Extratos Vegetais/análise , Extratos Vegetais/farmacocinética , Animais , Biotransformação , Limite de Detecção , Modelos Lineares , Masculino , Ratos , Ratos Sprague-Dawley , Reprodutibilidade dos Testes
7.
J Pharm Biomed Anal ; 166: 30-39, 2019 Mar 20.
Artigo em Inglês | MEDLINE | ID: mdl-30599279

RESUMO

Diabetic nephropathy (DN) is one of the leading causes of death in diabetes mellitus (DM). Early warning and therapy has significant clinical value for DN. This research sought to find biomarkers to predict the occurrence and development of DN and the intervention of Ginkgo biloba leaves extract (GBE) by quantifying fatty acids, amino acids, and nucleosides and nucleobases in rat plasma. Samples were respectively collected at the weekend of 5-10 weeks after diabetic rats induced by streptozotocin were defined. Plasma fasting blood-glucose, kidney index, blood urea nitrogen, creatinine, urine albumin excretion and ultrastructural morphology of kidney were measured or observed. Fatty acids, amino acids and nucleosides and nucleobases in rat plasma were analyzed by gas chromatography or liquid phase chromatography and mass spectrometry, respectively. From the biochemical index and morphological change of kidney, the rats from the 5th to 7th week were in the stage of DM while from the begin of 8th week the rats were suggested in the early stage of DN. The results of quantitative metabolomics showed that 16 differential metabolites were related to the progression of DN, and oleic acid, glutamate and guanosine might be the potential biomarkers of kidney injury. 14 differential metabolites were related to GBE against the progression of DN, while oleic acid and glutamate might be the potential biomarkers of GBE against kidney injury. Those findings potentially promote the understanding of the pathogenic progression of DN and reveal the therapeutic mechanism of GBE against DN.


Assuntos
Aminoácidos/sangue , Nefropatias Diabéticas/sangue , Ácidos Graxos/sangue , Metabolômica , Nucleosídeos/sangue , Extratos Vegetais/uso terapêutico , Albuminúria , Animais , Biomarcadores/sangue , Glicemia/metabolismo , Nitrogênio da Ureia Sanguínea , Creatinina/sangue , Diabetes Mellitus Experimental/sangue , Diabetes Mellitus Experimental/complicações , Diabetes Mellitus Experimental/tratamento farmacológico , Diabetes Mellitus Experimental/patologia , Nefropatias Diabéticas/complicações , Nefropatias Diabéticas/tratamento farmacológico , Rim/patologia , Rim/ultraestrutura , Masculino , Ratos
8.
J Sep Sci ; 42(5): 1105-1116, 2019 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-30575277

RESUMO

Methylation of the fifth carbon atom in cytosine is an epigenetic modification of deoxyribonucleic acid that plays important roles in numerous cellular processes and disease pathogenesis. Three additional states of cytosine, that is, 5-hydroxymethylcytosine, 5-formylcytosine and 5-carboxylcytosine, have been identified and associated with the diagnosis and/or prognosis of diseases. However, accurate measurement of those intermediates is a challenge since their global levels are relatively low. A number of innovative methods have been developed to detect and quantify these compounds in biological samples, such as blood, tissue and urine, etc. This review focuses on recent advancement in detection and quantification of four cytosine modifications, based on which, the development, diagnosis, and prognosis of diseases could be monitored through non-invasive procedures.


Assuntos
5-Metilcitosina/análise , 5-Metilcitosina/análogos & derivados , Animais , Cromatografia Líquida , Humanos , Espectrometria de Massas em Tandem
9.
Front Pharmacol ; 9: 1167, 2018.
Artigo em Inglês | MEDLINE | ID: mdl-30386241

RESUMO

Sangju Ganmao tablet (SGT), a well-known Chinese patent medicine used to treat cold symptoms, is made from eight herbal medicines. In this study, an off-line hydrophilic interaction × reversed-phase two-dimensional liquid chromatography (HILIC × RP 2D-LC) method was developed to comprehensively separate the chemical constituents of SGT. Through optimization of the experimental conditions, a total of 465 peaks were finally detected in SGT, and the structures of 54 selected compounds were fully identified or tentatively characterized by quadrupole time-of-flight mass spectrometry (qTOF-MS) analysis. The established 2D-LC analysis showed high orthogonality (63.62%) and approximate 11-fold improvement in peak capacity (2399 and 1099, obtained by two calculation methods), in contrast to conventional one-dimensional RPLC separation. The eight component herbs of SGT were also respectively separated by using the 2D-LC system, and we found that a total of 12 peaks detected in SGT were not discovered in any component herbs. These newly generated chemical constituents would benefit better understanding of the compatibility mechanism of the component herbs. The strategy established in this study could be used for systematic chemical comparison of SGT and its component herbs, which contributes to exploration of herbal compatibility mechanism.

10.
J Asian Nat Prod Res ; 20(7): 686-696, 2018 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-28349702

RESUMO

Ginsenosides F4 and Rg6 (GF4 and GRg6), two main active components of steamed notoginseng or red ginseng, are dehydrated disaccharide saponins. In this work, biotransformation of ginsenosides F4 and Rg6 in zebrafish was investigated by qualitatively identifying their metabolites and then proposing their possible metabolic pathways. The prediction of possible metabolism of ginsenosides F4 and Rg6 using zebrafish model which can effectively simulate existing mammals model was early and quickly performed. Metabolites of ginsenosides F4 and Rg6 after exposing to zebrafish for 24 h were identified by Ultraperformance Liquid Chromatography/Quadrupole-Time-of-Flight Mass Spectrometry. A total of 8 and 6 metabolites of ginsenosides F4 and Rg6 were identified in zebrafish, respectively. Of these, 7 and 5, including M1, M3-M5, M7-M9 and N1 (N5), N2, N4 (N9), N7-N8 were reported for the first time as far as we know. The mechanisms of their biotransformation involved were further deduced to be desugarization, glucuronidation, sulfation, dehydroxylation, loss of C-17 and/or C-23 residue pathways. It was concluded that loss of rhamnose at position C-6 and glucuronidation at position C-3 in zebrafish were considered as the main physiologic and metabolic processes of ginsenosides F4 and ginsenosides Rg6, respectively.

11.
Zhongguo Zhong Yao Za Zhi ; 42(20): 3996-4001, 2017 Oct.
Artigo em Chinês | MEDLINE | ID: mdl-29243439

RESUMO

UPLC-QTOF-MS/MS was used to identify metabolites in rat blood, urine and feces after the administration of n-butanol extract derived from steamed notoginseng. The metabolic process of saponins came from steamed notoginseng was analyzed. The metabolites were processed by PeakView software, and identified according to the structural characteristics of prototype compounds and the accurate qualitative and quantitative changes of common metabolic pathways. Four saponins metabolites were identified based on MS/MS information of metabolites, namely ginsenoside Rh4, Rk3, Rk1, Rg5,and their 15 metabolites were verified. The metabolic pathways of the four ginsenosides in n-butanol extract included glucuronidation, desugar, sulfation, dehydromethylation, and branch loss. The metabolites of main active saponin components derived from steamed Panax notoginseng were analyzed from the perspective of qualitative analysis. And the material basis for the efficacy of steamed notoginseng was further clarified.

12.
J Pharm Biomed Anal ; 146: 68-78, 2017 Nov 30.
Artigo em Inglês | MEDLINE | ID: mdl-28854404

RESUMO

Ginkgo biloba extract (GBE), derived from the leaves of Ginkgo biloba L., is one of the most widely used traditional Chinese medicines worldwide. Due to high structural diversity and low abundance of chemical constituents in GBE, conventional reversed-phase liquid chromatography has limited power to meet the needs of its quality control. In this study, an off-line hydrophilic interaction×reversed-phase two-dimensional liquid chromatography (HILIC×RP 2D-LC) system coupled with diode array detection (DAD) and quadrupole time-of-flight mass spectrometry (qTOF-MS) was established to comprehensively analyze the chemical constituents of GBE. After optimizing the chromatographic columns and mobile phase of 2D-LC, a Waters XBridge Amide column using acetonitrile/water/formic acid as the mobile phase was selected as the first dimension to fractionate GBE, and the obtained fractions were further separated on an Agilent Zorbax XDB-C18 column with methanol/water/formic acid as the mobile phase. As a result, a total of 125 compounds were detected in GBE. The orthogonality of the 2D-LC system was 69.5%, and the practical peak capacity was 3864 and 2994, respectively, calculated by two different methods. The structures of 104 compounds were tentatively characterized by qTOF-MS analysis, and 21 of them were further confirmed by comparing with reference standards. This established HILIC×RP 2D-LC-qTOF/MS system can greatly improve the separation and characterization of natural products in GBE or other complicated herbal extracts.


Assuntos
Medicamentos de Ervas Chinesas/química , Ginkgo biloba/química , Extratos Vegetais/química , Acetonitrilos/química , Cromatografia Líquida de Alta Pressão/métodos , Cromatografia de Fase Reversa/métodos , Flavonoides/química , Formiatos/química , Interações Hidrofóbicas e Hidrofílicas , Medicina Tradicional Chinesa/métodos , Folhas de Planta/química , Espectrometria de Massas por Ionização por Electrospray/métodos , Água/química
13.
J Chromatogr Sci ; 55(3): 334-345, 2017 03 01.
Artigo em Inglês | MEDLINE | ID: mdl-27913377

RESUMO

Chromatographic separation is still a critical subject for the quality control of traditional Chinese medicine. In this study, three different high performance liquid chromatographic (HPLC) systems employing commercially available columns packed with 1.8, 3.5 and 5.0 µm particles were respectively developed and optimized for the combinative fingerprint analysis and multi-ingredients quantification of Sangju Ganmao tablet (SGT). Chromatographic parameters including the repeatability of retention time and peak area, symmetry factor, resolution, number of theoretical plates and peak capacity were used to assess the chromatographic performance of different HPLC systems. The optimal chromatographic system using Agilent ZORBAX SB-C18 column (2.1 mm × 100 mm, 3.5 µm) as stationary phase was respectively coupled with diode array detector or mass spectrometry detector for the chromatographic fingerprint analysis and simultaneous quantification or identification of nine compounds of SGT. All the validation data conformed to the acceptable requirements. For the fingerprint analysis, 31 peaks were selected as the common peaks to evaluate the similarities of SGT from 10 different manufacturers using heatmap, hierarchical cluster analysis and principal component analysis. The results demonstrated that the combinations of the quantitative and chromatographic fingerprint analysis offer an efficient way to evaluate the quality consistency of SGT.


Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Medicamentos de Ervas Chinesas/química , Espectrometria de Massas/métodos , Análise por Conglomerados , Limite de Detecção , Modelos Lineares , Análise de Componente Principal , Reprodutibilidade dos Testes , Comprimidos
14.
Biomed Chromatogr ; 31(4)2017 Apr.
Artigo em Inglês | MEDLINE | ID: mdl-27696453

RESUMO

As essential endogenous compounds, nucleobases and nucleosides fulfill various functions in living organisms. This study presents the development and validation of a new hydrophilic interaction liquid chromatography tandem mass spectrometry method for simultaneous quantification of 19 nucleobases and nucleosides in rat plasma. For the sample preparation, 15 kinds of protein precipitants were evaluated according to the chromatographic profile and ion response of analytes. The optimization of chromatographic separation was respectively performed using reversed-phase liquid chromatography and hydrophilic interaction liquid chromatography mode; each separation mode included two test columns with different stationary phases. The chromatographic profile and parameters such as half-width (W1/2 ), capacity factor (K') and tailing factor (ft ) were used to evaluate the separation efficiencies. Furthermore, the adopted composition of two mobile phase systems and the concentrations of the additives in the optimum buffer system were also investigated. The developed method was fully validated and successfully applied quantitatively to determine 19 nucleobases and nucleosides in plasma from normal and diabetic nephropathy (DN) rats. Significant differences between normal and DN rats were found in plasma levels of cytosine, xanthine, thymidine, adenosine, guanosine, inosine and 8-hydroxy-2'-deoxyguanosine. This information may provide a useful reference for the discovery of potential biomarkers of DN.


Assuntos
Cromatografia Líquida/métodos , Nucleosídeos/sangue , Espectrometria de Massas em Tandem/métodos , Adenina/sangue , Animais , Cromatografia de Fase Reversa/métodos , Citosina/sangue , Desoxiguanosina/análogos & derivados , Desoxiguanosina/sangue , Nefropatias Diabéticas/sangue , Interações Hidrofóbicas e Hidrofílicas , Pirimidinas/sangue , Ratos Sprague-Dawley , Reprodutibilidade dos Testes , Espectrometria de Massas em Tandem/normas , Xantina/sangue
15.
J Chromatogr Sci ; 54(4): 625-32, 2016 Apr.
Artigo em Inglês | MEDLINE | ID: mdl-26809640

RESUMO

A simple and sensitive liquid chromatography method with diode array detector was established for simultaneous determination of 11 components (geniposidic acid, chlorogenic acid, caffeic acid, geniposide, luteoloside, isochlorogenic acid C, baicalin, luteolin, wogonoside, baicalein and wogonin) in various commercial Yinzhihuang preparations and their herbs by optimizing the extraction, separation and analytical conditions. Eleven components were identified on the basis of their retention times and mass spectra. Chromatographic separation was performed on a C18 analytical column with a gradient elution of acetonitrile and 0.1% formic acid water solution at a flow rate of 1.0 mL/min. The linearity, precision and accuracy of the data obtained were acceptable. The method was used to analyze four Yinzhihuang preparations (powder, capsule, oral liquid and injection) and related herbs (Radix Scutellariae, Flos Lonicerae, Herba Artemisiae Scopariae and Fructus gardeniae). Results suggested that the optimized method could be considered as a good approach to control the quality of Yinzhihuang preparations and their herbs.


Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Medicamentos de Ervas Chinesas/química , Espectrofotometria Ultravioleta/métodos , Reprodutibilidade dos Testes
16.
J Sep Sci ; 39(1): 21-37, 2016 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-26347023

RESUMO

Two-dimensional liquid chromatography has become an attractive analytical tool for the separation of complex samples due to its enhanced selectivity, peak capacity, and resolution compared with one-dimensional liquid chromatography. Recently, more attention has been drawn on the application of this separation technique in studies concerning traditional Chinese medicines, metabonomes, proteomes, and other complex mixtures. In this review, we aim to examine the application of two-dimensional liquid chromatography in traditional Chinese medicine analysis and metabonomic investigation. The classification and evaluation indexes were first introduced. Then, various switching methods were summarized when used in an on-line two-dimensional liquid chromatography system. Finally, the applications of this separation technique in traditional Chinese medicine analysis and metabonomic investigation were discussed on the basis of specific studies.


Assuntos
Cromatografia Líquida/métodos , Medicamentos de Ervas Chinesas/análise , Metabolômica/métodos , Humanos , Medicina Tradicional Chinesa
17.
Mass Spectrom Rev ; 35(5): 574-600, 2016 09.
Artigo em Inglês | MEDLINE | ID: mdl-25284160

RESUMO

Hydrophilic interaction chromatography (HILIC) is an emerging separation mode of liquid chromatography (LC). Using highly hydrophilic stationary phases capable of retaining polar/ionic metabolites, and accompany with high organic content mobile phase that offer readily compatibility with mass spectrometry (MS) has made HILIC an attractive complementary tool to the widely used reverse-phase (RP) chromatographic separations in metabolomic studies. The combination of HILIC and RPLC coupled with an MS detector expands the number of detected analytes and provides more comprehensive metabolite coverage than use of only RP chromatography. This review describes the recent applications of HILIC-MS/MS in metabolomic studies, ranging from amino acids, lipids, nucleotides, organic acids, pharmaceuticals, and metabolites of specific nature. The biological systems investigated include microbials, cultured cell line, plants, herbal medicine, urine, and serum as well as tissues from animals and humans. Owing to its unique capability to measure more-polar biomolecules, the HILIC separation technique would no doubt enhance the comprehensiveness of metabolite detection, and add significant value for metabolomic investigations. © 2014 Wiley Periodicals, Inc. Mass Spec Rev 35:574-600, 2016.


Assuntos
Cromatografia Líquida , Interações Hidrofóbicas e Hidrofílicas , Metabolômica , Animais , Cromatografia de Fase Reversa , Humanos , Espectrometria de Massas em Tandem
18.
Curr Drug Metab ; 17(4): 386-400, 2016.
Artigo em Inglês | MEDLINE | ID: mdl-26651973

RESUMO

During the development, dosage optimization and safety evaluation of a drug, rapid and precise monitoring of administered drug and/or its metabolites in biological samples including blood, plasma, serum, tissues and saliva are vital. As drug biotransformation produces more hydrophilic metabolites for the enhancement of drug elimination, which is often a challenge for traditional reversed-phase liquid chromatography (RPLC) separation. Because hydrophilic interaction liquid chromatography (HILIC) is capable of retaining polar compounds and readily compatible with mass spectrometry (MS), HILIC has been used as a complementary separation technique to RPLC for analysis of polar metabolites, especially polar drugs and their metabolites. This review covers core aspects of HILIC-MS/MS method and overall profile of its application in analysis of drug and/or its metabolites. The emphasis of this paper has been placed on the applications of HILIC-MS/MS method in quantitative bioanalysis of drugs alone or along with their metabolites in drug metabolism studies in recent years. As a fundamental and critical step of bioanalytical method, conventional sample preparation techniques of biological matrices for the HILIC-MS/MS analysis of drugs and/or their metabolites are also briefly featured.


Assuntos
Cromatografia Líquida/métodos , Preparações Farmacêuticas/análise , Preparações Farmacêuticas/metabolismo , Espectrometria de Massas em Tandem/métodos , Analgésicos/análise , Analgésicos/metabolismo , Métodos Analíticos de Preparação de Amostras , Antibacterianos/análise , Antibacterianos/metabolismo , Anticarcinógenos/análise , Anticarcinógenos/metabolismo , Antivirais/análise , Antivirais/metabolismo , Humanos , Interações Hidrofóbicas e Hidrofílicas , Inativação Metabólica
19.
Artigo em Inglês | MEDLINE | ID: mdl-26113453

RESUMO

The mesangial cell (MC) cultured with high glucose has been used to observe the protective effect of Ginkgo biloba extract (GBE) against diabetic nephropathy (DN), but the compounds interacting with cell are still unknown, which may be potential bioactive components. Based on this, the determination of GBE in MC lysates was proposed by high performance liquid chromatography tandem mass spectrometry (LC-MS/MS) in this study. The MC was cultured with normal or high glucose with GBE for 4, 8, 12, 16, 24 and 48h. The harvested cell was extracted with 40% acetic acid in water and further analyzed by LC-MS/MS. All the validation data including linearity, intra-day and inter-day precision, limit of detection and quantification, matrix effect, and stability were within the required limits. The validated method was successfully applied to quantify 11 compounds of GBE in cell lysates. The results showed that high glucose prolonged the peak time of all observed 11 compounds and peak concentrations of bilobalide, ginkgolide C, ginkgolide B, quercetin, luteolin, kaempferol, isorhamnetin and genkwanin in cell lysates, which hinted that these compounds may be the potential bioactive components of GBE with preventive effect against DN.


Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Ginkgo biloba/química , Células Mesangiais/metabolismo , Extratos Vegetais/análise , Extratos Vegetais/metabolismo , Espectrometria de Massas em Tandem/métodos , Técnicas de Cultura de Células , Nefropatias Diabéticas , Glucose/metabolismo , Humanos , Reprodutibilidade dos Testes
20.
Chem Commun (Camb) ; 51(42): 8880-3, 2015 May 25.
Artigo em Inglês | MEDLINE | ID: mdl-25925958

RESUMO

A sensitive and selective strategy for the colorimetric visualization of the total monomeric Aß down to 40 pg mL(-1) based on dual-functionalized gold nanoplasmonic particles (GNPs) is developed and applied to evaluate Aß levels in the AD cerebral system.


Assuntos
Doença de Alzheimer/diagnóstico , Doença de Alzheimer/metabolismo , Peptídeos beta-Amiloides/análise , Encéfalo/metabolismo , Colorimetria , Ouro/química , Nanopartículas Metálicas/química , Peptídeos beta-Amiloides/metabolismo , Animais , Nanopartículas Metálicas/análise , Estrutura Molecular , Tamanho da Partícula , Ratos , Propriedades de Superfície
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