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1.
Carcinogenesis ; 2024 Feb 02.
Artigo em Inglês | MEDLINE | ID: mdl-38306794

RESUMO

Hepatocellular carcinoma (HCC) exhibits a high mortality rate due to its high invasion and metastatic nature, and the acidic microenvironment plays a pivotal role. Acid-sensing ion channel 1 (ASIC1) is upregulated in HCC tissues and facilitates tumor progression in a pH-dependent manner, while the specific mechanisms therein remain currently unclear. Herein, we aimed to investigate the underlying mechanisms by which ASIC1 contributes to the development of HCC. Using bioinformatics analysis, we found a significant association between ASIC1 expression and malignant transformation of HCC, such as poor prognosis, metastasis and recurrence. Specifically, ASIC1 enhanced the migration and invasion capabilities of Li-7 cells in the in vivo experiment using an HCC lung metastasis mouse model, as well as in the in vitro experiments such as wound healing assay and Transwell assay. Furthermore, our comprehensive gene-chip and molecular biology experiments revealed that ASIC1 promoted HCC migration and invasion by activating the PRKACA/AP-1 signaling pathway. Our findings indicate that targeting ASIC1 could have therapeutic potential for inhibiting HCC progression.

2.
Am J Cancer Res ; 13(5): 1718-1743, 2023.
Artigo em Inglês | MEDLINE | ID: mdl-37293163

RESUMO

Recurrence and metastasis are major factors associated with the poor prognosis of pancreatic cancer (PC). Previous studies have indicated that METTL3-mediated N6-methyladenosine (m6A) modification is closely associated with PC progression and prognosis. However, its underlying regulatory mechanisms remain unclear. In this study, we found that METTL3 was upregulated in PC tissues and cells and was associated with malignant tumor progression and poor progression-free survival in PC. Linc00662 was screened as a m6A-enriched RNA that promoted tumor growth and metastasis in PC cells and mouse models and was associated with poor clinical prognosis. Four m6A motifs were identified in Linc00662, which maintained the stability of Linc00662 in an IGF2BP3-coupled manner and were closely associated with the pro-tumor properties of Linc00662 in vitro and in vivo. ITGA1 was identified as a downstream gene regulated by Linc00662. Linc00662 recruites GTF2B to activate the transcription of ITGA1 in a m6A-dependent manner and initiates the formation of focal adhesions through the ITGA1-FAK-Erk pathway, thereby promoting malignant behavior in PC cells. The FAK inhibitor-Y15 obviously repressed tumor progression in Linc00662-overexpressing PC cells in vitro and in vivo. This study proposes a novel regulatory mechanism of Linc00662 in oncogene activation in PC and indicates that Linc00662 and its downstream genes are potential targets for PC therapy.

3.
J Gastrointest Oncol ; 12(5): 2325-2333, 2021 Oct.
Artigo em Inglês | MEDLINE | ID: mdl-34790395

RESUMO

BACKGROUND: Recurrence and metastasis are the major causes of pancreatic ductal adenocarcinoma (PDAC) mortality after treatment. The underlying molecular mechanism is poorly understood. Actin-related protein 3 (ACTR3) is an important component of the actin-related protein 2/3 complex, which is involved in the regulation of cell motility and epithelial mesenchymal transition (EMT) process. Previously published studies have indicated that ACTR3 expression is upregulated in several types of cancers, and promotes tumor development, including gastric cancer and hepatocellular carcinoma. However, to date, the expression levels and the role of ACTR3 in PDAC are not well understood. METHODS: In the present study, the expression levels of ACTR3 in PDAC tissue and the relationship of ACTR3 expression with clinical prognosis were analyzed by mRNA microarray and bioinformatics. The biological functions and underlying mechanism of ACTR3 in PDAC were examined by a series of assays, including Cell Counting Kit-8 (CCK-8), transwell assay, and Western blotting. RESULTS: We found that the expression of ACTR3 was significantly increased in PDAC tissues and cell lines. A higher expression of ACTR3 was predictive of poor outcome for patients with PDAC. In vitro, the knockdown of ACTR3 expression significantly inhibited the invasive and migratory capacity of PDAC cells, and altered the distribution of F-actin and the expression of EMT markers. CONCLUSIONS: The findings of our study indicated that ACTR3 promotes cell migration and invasion by inducing EMT in PDAC, which may be a potential therapeutic target and prognostic indicator for PDAC patients.

4.
J Cancer ; 12(18): 5622-5632, 2021.
Artigo em Inglês | MEDLINE | ID: mdl-34405022

RESUMO

Background: Although we previously revealed that DNA-dependent protein kinase catalytic subunit (DNA-PKcs) is overexpressed in pancreatic ductal adenocarcinoma (PDAC) and important for gemcitabine resistance, the role of DNA-PKcs in the progression and metastasis of PDAC remain unclear. To date, the upstream signaling events stimulating DNA-PKcs overexpression in PDAC are still not well characterized. Methods: Expression of DNA-PKcs was measured by western blot. The levels of miRNA-101 and lncRNA nuclear paraspeckle assembly transcript 1 (NEAT1) were detected by real-time PCR. Cell viability was determined by CCK-8. Cell migration and cell invasion were measured by transwell assay. The regulatory relationship between NEAT1 and miR-101 was determined by a luciferase assay. Results: DNA-PKcs expression was significantly elevated in human PDAC tissues and cells. DNA-PKcs overexpression was correlated with TNM stage and lymph node metastasis. Higher expression of DNA-PKcs was closely correlated with patients of worse overall survival (OS). DNA-PKcs knockdown suppresses malignant behaviors of PDAC cells. Further study showed that miRNA-101 level was decreased in PDAC tissues and cells, which could be responsible for DNA-PKcs overexpression and DNA-PKcs mediated oncogenic actions in PDAC cells. Moreover, NEAT1 functions as an oncogene influencing cell proliferation, migration and invasion in part by serving as a competing endogenous RNA (ceRNAs) modulating miR-101 expression, leading to up-regulation of DNA-PKcs. Conclusion: These findings suggest that NEAT1/miR-101-dependent up-regulation of DNA-PKcs promotes the malignant behaviors of PDAC cells. The NEAT1/miR-101/DNA-PKcs axis may serve as a viable prognostic marker and therapeutic target for PDAC.

5.
Front Biosci (Landmark Ed) ; 23(2): 388-396, 2018 01 01.
Artigo em Inglês | MEDLINE | ID: mdl-28930552

RESUMO

Available evidence suggests that autophagy may serve as a tumor suppressor in cases of chronic liver disease and liver cirrhosis and that autophagic deficiency may lead to hepatocellular carcinoma (HCC). Recent studies suggested that the development of several tumor types could be regulated by microRNA-181a. However, the role of miR-181a in the autophagy of HCC remains unclear. In this study, we aimed to investigate the role of miR-181a in the autophagy of HCC. We found that the mRNA expression of miR-181a is higher but the level of autophagy is lower in human HCC compared to normal liver tissue. A luciferase assay confirmed that Atg5 is the target gene of miR-181a. Moreover, the results showed that an miR-181a sponge increased apoptosis in HepG2 cells and reduced the growth of tumors in a HepG2 cell xenograft tumor model. In conclusion, these results suggest that miR-181a can inhibit autophagy in HCC by targeting Atg5, resulting in decreased apoptosis of HCC cells and increased tumor growth.


Assuntos
Proteína 5 Relacionada à Autofagia/genética , Autofagia/genética , Carcinoma Hepatocelular/genética , Regulação Neoplásica da Expressão Gênica , Neoplasias Hepáticas/genética , MicroRNAs/genética , Regiões 3' não Traduzidas/genética , Animais , Apoptose/genética , Carcinoma Hepatocelular/patologia , Células Hep G2 , Humanos , Neoplasias Hepáticas/patologia , Camundongos Endogâmicos BALB C , Camundongos Nus , Transplante Heterólogo , Carga Tumoral/genética
6.
J Chromatogr A ; 1217(49): 7807-11, 2010 Dec 03.
Artigo em Inglês | MEDLINE | ID: mdl-21035121

RESUMO

An integrative coupling method of headspace liquid-phase microextraction (HS-LPME) and capillary zone electrophoresis (CZE) was proposed in this paper. In the method, a separation capillary was used to create a microextraction droplet of the running buffer solution of CZE, hold the droplet at the capillary inlet, extract analytes of sample solutions in the headspace of a sample vial, inject concentrated analytes into the capillary and separate the analytes by CZE. The proposed method was applied to determine the preservatives of benzoic acid and sorbic acid in soy sauce and soft drink samples, in which the running buffer solution of 50 mmol/L tetraborate (pH 9.2) was directly used to form the acceptor droplet at the capillary inlet by pressure, and the preservatives in a 6-mL sample solution containing 0.25 g/mL NaCl were extracted at 90°C for 30 min in the headspace of a 14-mL sample vial. Then the concentrated preservatives were injected into the capillary at 10 cm height difference for 20 s and separated by CZE. The enrichment factors of benzoic acid and sorbic acid achieved 266 and 404, and the limits of detection (LODs) were 0.03 and 0.01 µg/mL (S/N=3), respectively. The recoveries were in the range of 88.7-105%. The integrative coupling method of HS-LPME and CZE was simple, convenient, reliable and suitable for concentrating volatile and semi-volatile organic acids and eliminating matrix interferences of real samples.


Assuntos
Ácido Benzoico/análise , Fracionamento Químico/métodos , Eletroforese Capilar/métodos , Conservantes de Alimentos/análise , Ácido Sórbico/análise , Concentração de Íons de Hidrogênio , Cloreto de Sódio , Temperatura , Fatores de Tempo
7.
J Hazard Mater ; 184(1-3): 331-336, 2010 Dec 15.
Artigo em Inglês | MEDLINE | ID: mdl-20828927

RESUMO

An electrochemical hydride generation system with polyaniline-modified lead cathode was developed for tin determination by coupling with atomic fluorescence spectrometry. The tin fluorescence signal intensity was improved evidently as the polyaniline membrane could facilitate the transformation process from atomic tin to the SnH(4) and prevent the aggradation of Sn atom on Pb electrode surface. The effects of experimental parameters and interferences have been studied. The limit of detection (LOD) was 1.5 ng mL(-1) (3σ) and the relative standard deviation (RSD) was 3.3% for 11 consecutive measurements of 50 ng mL(-1) Sn(IV) standard solution.


Assuntos
Compostos de Anilina/química , Eletroquímica/métodos , Eletrodos , Análise de Alimentos/métodos , Hidrogênio/química , Chumbo/química , Espectrometria de Fluorescência/métodos , Estanho/análise
8.
Guang Pu Xue Yu Guang Pu Fen Xi ; 30(3): 762-6, 2010 Mar.
Artigo em Chinês | MEDLINE | ID: mdl-20496704

RESUMO

In the present paper, a laboratory-made high-performance electrophoresis microcolumn unit was prepared for UV-Vis spectrophotometer. X-ray diffraction was used in the preparation of electrophoretic microcolumns. And an analytical technique of microcolumn electrophoresis coupled with UV-Vis spectrophotometry was introduced. Uniform quartz microncrystals were prepared by hydrothermal synthesis. Their crystalline phase and morphology were identified by X-ray diffraction and scanning electron microscope, respectively. The quartz microncrystals were packed into a 2-mm i. d. fused-silica tube to prepare the electrophoretic microcolumn. With 1.5 mmol x L(-1) disodium phosphate buffer solution (pH 11.5) containing 25% (phi) methanol and 10% (phi) acetonitrile, tryptophan, phenylalanine and tyrosine were on-line separated on line and detected by microcolumn electrophoresis coupled with UV-Vis spectrophotometry without derivatization. The limits of detection were 0.037, 0.20 and 0.20 micromol x L(-1), respectively. The separation efficiency of tryptophan was 4.5 x 10(4) plates/m. The sample capacity of the electrophoretic microcolumn achieved 35 microL. It was found that the electrophoretic microcolumn packed with quartz microncrystals was able to limit Joule heat, increase sample capacity and enhance detection sensitivity. The laboratory-made electrophoretic microcolumn could be a high-performance separation unit for conventional UV-Vis spectrophotometer. The on-line coupling of microcolumn electrophoresis and UV-Vis spectrophotometry could separate and determine samples with complicated matrices, reduce zone broadening and enhance separation efficiency, so expand the analytical function of spectrophotometer in the trace analysis of mixed components with overlapped spectra.

9.
J Chromatogr A ; 1217(8): 1203-7, 2010 Feb 19.
Artigo em Inglês | MEDLINE | ID: mdl-20034631

RESUMO

An analytical technique of in-line coupling headspace liquid-phase microextraction (HS-LPME) with capillary electrophoresis (CE) was proposed to determine volatile analytes. A special cover unit of the sample vial was adopted in the coupling method. To evaluate the proposed method, phenols were used as model analytes. The parameters affecting the extraction efficiency were investigated, including the configuration of acceptor phase, kind and concentration of acceptor solution, extraction temperature and time, salt-out effect, sample volume, etc. The optimal enrichment factors of HS-LPME were obtained with the sample volume of about half of sample vials, which were confirmed by both the theoretical prediction and experimental results. The enrichment factors were obtained from 520 to 1270. The limits of detection (LODs, S/N=3) were in the range from 0.5 to 1 ng/mL each phenol. The recoveries were from 87.2% to 92.7% and the relative standard deviations (RSDs) were lower than 5.7% (n=6). The proposed method was successfully applied to the quantitative analysis of the phenols in tap water, and proved to be a simple, convenient and reliable sample preconcentration and determination method for volatile analytes in water samples.


Assuntos
Fracionamento Químico/instrumentação , Eletroforese Capilar/métodos , Água Doce/análise , Fenóis/análise , Poluentes Químicos da Água/análise , Fracionamento Químico/métodos , Desenho de Equipamento , Limite de Detecção , Fenóis/isolamento & purificação , Poluentes Químicos da Água/isolamento & purificação
10.
Talanta ; 79(2): 314-8, 2009 Jul 15.
Artigo em Inglês | MEDLINE | ID: mdl-19559884

RESUMO

An integrated electrochemical hydride generation cell, mainly composed of three components (a gas liquid separator, a graphite tube cathode and a reticulate Pt wire anode), was laboratory constructed and employed for the detection of arsenic by coupling to atomic fluorescence spectrometry. This integrated cell was free of ion-exchange membrane and individual anolyte, with the virtues of low-cost, easy assembly and environmental-friendly. Using flow injection mode, the sample throughput could come to 120 h(-1) attributed to the small dimension of the cathode chamber. The operating conditions for the electrochemical hydride generation of arsenic were investigated in detail and the potential interferences from oxygen or various ions were also evaluated. Under the optimized conditions, no obvious oxygen quenching effects were observed. The limit of detection of As (III) for the sample blank solution was 0.2 ng mL(-1) (3sigma) and the relative standard deviation was 3.1% for nine consecutive measurements of 5 ng mL(-1) As (III) standard solution. The calibration curve was linear up to 100 ng mL(-1). The accuracy of the method was verified by the determination of arsenic in the reference materials GBW08517 (Laminaria Japonica Aresch) and GBW10023 (Porphyra crispata) and the developed method was successfully applied to determine trace amounts of arsenic in edible seaweeds.


Assuntos
Arsênio/análise , Técnicas Eletroquímicas/métodos , Alga Marinha/química , Espectrofotometria Atômica/métodos , Calibragem , Técnicas Eletroquímicas/normas , Hidrogênio/química , Oxigênio , Padrões de Referência
11.
Talanta ; 79(2): 460-5, 2009 Jul 15.
Artigo em Inglês | MEDLINE | ID: mdl-19559905

RESUMO

The feasibility of a microcolumn electrophoresis technique was investigated with a 100mm length, 2mm I.D. fused-silica microcolumn packed with uniform quartz microncrystals prepared by hydrothermal synthesis. To evaluate the separation technique, tryptophan, phenylalanine and tyrosine were primarily separated by the microcolumn electrophoresis and detected at 216 nm without derivatization by an ordinary spectrophotometer. The separation conditions of the amino acids were optimized. With 1.5 mmol/L disodium phosphate buffer solution (pH 11.5) containing 25% (v/v) methanol and 10% (v/v) acetonitrile, the three amino acids were separated and the separation efficiency of tryptophan was 4.5x10(4)plates/m. The limits of detection were 0.035, 0.22 and 0.20 micromol/L, respectively. The sample capacity of the electrophoretic microcolumn achieved 35 microL. The proposed method was used to determine these amino acids in compound amino acid injection samples without derivatization. For the simplicity and portability of the microcolumn electrophoresis, it is studied as one of the high-performance separation techniques for an in situ and real-time electrokinetic flow analysis system. For its high detection sensitivity and large sample capacity, it can be developed for preparative electrophoresis.


Assuntos
Eletroforese Capilar/instrumentação , Aminoácidos Aromáticos/isolamento & purificação , Eletroforese Capilar/métodos , Eletroforese Capilar/normas , Métodos , Quartzo , Espectrofotometria Ultravioleta
12.
J Chromatogr A ; 1216(20): 4504-9, 2009 May 15.
Artigo em Inglês | MEDLINE | ID: mdl-19329123

RESUMO

A wall-free detection method based on liquid junction in a capillary gap was proposed for laser-induced fluorescence (LIF) of capillary electrophoresis (CE). The capillary gap of the wall-free cell was fabricated by etching a 10-mm x 50-microm I.D. fused-silica capillary to obtain a polyimide coating sleeve, decoating about 6mm at one end of both 50 microm I.D. separation and liquid junction capillary, inserting the treated capillary ends into the coating sleeve oppositely, fixing the capillaries with a gap distance of 140 microm by epoxy glue and removing the coating sleeve by burning. The theoretical model, experimental results and wall-free cell images indicated that the gap distance and applied voltage were main influence factors on the wall-free detection. Since the wall-free cell increased the absorption light path and avoided the stray light from the capillary wall, it improved the ratio of signal to noise and limit of detection (LOD) of CE-LIF. Three flavin compounds of riboflavin (RF), flavin mononucleotide sodium (FMN) and flavin adenine dinucleotide disodium (FAD) were used to evaluate the wall-free detection method. Compared with on-column cell, the LODs of the wall-free cell were improved 15-, 6- and 9-fold for RF, FMN and FAD, respectively. The linear calibration concentrations of the flavins ranged from 0.005 to 5.0 micromol/L. The column efficiency was in the range from 1.0 x 10(5) to 2.5 x 10(5) plates. The wall-free detection of CE-LIF was applied to the analysis of the flavins in spinach and lettuce leaves.


Assuntos
Eletroforese Capilar/instrumentação , Flavinas/química , Eletroforese Capilar/métodos , Fluorescência , Lasers , Sistemas On-Line , Verduras/química
13.
J Chromatogr A ; 1216(15): 3353-9, 2009 Apr 10.
Artigo em Inglês | MEDLINE | ID: mdl-19203764

RESUMO

A simple and efficient dual preconcentration method of on-column liquid-liquid-liquid microextraction (LLLME) coupled with base stacking was developed for capillary zone electrophoresis (CZE) in this paper. Four N-methyl carbamates were used as target compounds to evaluate the enrichment means. The carbamates in sample solutions (donor phase) were extracted into a dodecanol phase immobilized on a porous hollow fiber, hydrolyzed and back extracted into 0.20 microL running buffer (acceptor phase) of 30 mmol/L methylamine hydrochloride (pH 11.6) containing 0.5 mmol/L tetradecyltrimethylammonium bromide inside the hollow fiber, stacked further with 0.5 mol/L NaOH injected at -10 kV for 60s, and separated by CZE. Analytical parameters affecting the LLLME, base stacking and CZE were investigated, including sample solution volume, pH and temperature, extraction time, stirring rate, buffer component, buffer pH, NaOH concentration, stacking time, etc. The enrichment factors of the carbamates were higher than 1100. The relative standard deviation (RSD) of peak height and limits of detection (LODs) were 4.5-5.5% (n=6) and 2-4 ng/mL (S/N=3) for standard solutions, respectively. The proposed method was applied to the analysis of vegetable and fruit samples with the RSD less than 6.0% (n=3) and LODs of 6-10 ng/g (S/N=3). The calibration solutions were prepared by diluting the stock solutions with blank sample solutions, and the calibration concentrations ranged from 0.012 to 1.0 microg/mL (r>0.9951). The analytical results demonstrated that the LLLME coupled with base stacking was a simple, convenient and reliable on-column sample pretreatment method for the analysis of anionic analytes in CZE.


Assuntos
Carbamatos/análise , Fracionamento Químico/métodos , Eletroforese Capilar/métodos , Resíduos de Praguicidas/análise , Frutas/química , Concentração de Íons de Hidrogênio , Hidrólise , Reprodutibilidade dos Testes , Sensibilidade e Especificidade , Hidróxido de Sódio/química , Temperatura , Verduras/química
14.
Artigo em Inglês | MEDLINE | ID: mdl-19117808

RESUMO

An analytical method for kanamycin A, amikacin and tobramycin of aminoglycoside (AG) antibiotics in milk samples was proposed using capillary zone electrophoresis (CZE) with post-column derivatization and laser-induced fluorescence detection. A simple and convenient homemade coaxial-gap reactor was adopted in the post-column derivatization of the AGs with 1.0 mmol/L naphthalene-2,3-dicarboxaldehyde and 8.0 mmol/L 2-mercaptoethanol in 35 mmol/L sodium tetraborate buffer (pH 10.0) of 30% (v/v) methanol. 50 mmol/L sodium acetate (pH 5.0) containing 0.5 mmol/L cetyltrimethyl ammonium bromide was used as the separation buffer. The linear calibration concentrations and detection limits were from 2.1 x 10(-5) to 5.0 x 10(-2)g/L and in the range of 7 x 10(-6) to 2 x 10(-5)g/L, respectively. The recoveries of the AGs in milk samples were from 81.6 to 93.1% (n=3).


Assuntos
Amicacina/análise , Resíduos de Drogas/análise , Eletroforese Capilar , Canamicina/análise , Leite/química , Tobramicina/análise , Animais , Antibacterianos/análise , Eletroforese Capilar/instrumentação , Eletroforese Capilar/métodos , Fluorescência , Concentração de Íons de Hidrogênio , Modelos Lineares , Sensibilidade e Especificidade
15.
Anal Chim Acta ; 618(1): 79-85, 2008 Jun 16.
Artigo em Inglês | MEDLINE | ID: mdl-18501248

RESUMO

An electrokinetic flow analysis system (EFA), consisting of one electroosmotic pump, five solenoid valves and one on-line homemade solid phase extraction (SPE) unit, combined with capillary zone electrophoresis (CZE) was proposed to determine benzoic acid and sorbic acid in food products. Tetrabutylammonium bromide (TBAB) was adopted as an ion pair reagent to improve the retention of the preservatives on C(8)-bonded silica sorbent, which was also used to remove sample matrices. By using the SPE unit, the EFA-SPE-CZE system was able to perform the SPE operation and CZE separation simultaneously. With a modified interface of EFA and CZE, the buffer consumption was reduced to 130 microL for each running. The preservatives were separated and determined under optimized conditions with p-hydroxybenzoic acid as an internal standard. The relative standard deviation (R.S.D.) of peak area for each analyte was less than 3.1% (n=5) and the limits of detection (LODs) ranged from 10 to 20 ngmL(-1) (K=3, n=11).


Assuntos
Ácido Benzoico/análise , Frutas/química , Glycine max/química , Leite/química , Extração em Fase Sólida/métodos , Ácido Sórbico/análise , Animais , Bebidas , Eletroquímica , Eletroforese Capilar/instrumentação , Eletroforese Capilar/métodos , Análise de Injeção de Fluxo/instrumentação , Análise de Injeção de Fluxo/métodos , Análise de Alimentos/instrumentação , Análise de Alimentos/métodos , Cinética , Reprodutibilidade dos Testes , Sensibilidade e Especificidade , Extração em Fase Sólida/instrumentação , Fatores de Tempo
16.
Talanta ; 74(5): 1371-7, 2008 Feb 15.
Artigo em Inglês | MEDLINE | ID: mdl-18371792

RESUMO

A convenient and automated method for on-line pretreatment and determination of three parabens (i.e. methyl, ethyl and propyl p-hydroxybenzoate) in cosmetic products is proposed by using flow injection analysis (FIA), solid-phase extraction (SPE) and micellar electrokinetic chromatography (MEKC). An improved split-flow interface is used to couple SPE on C(8)-bonded silica with MEKC separation, which can avoid running buffer contamination and reduce buffer consumption, especially, containing expensive reagents. The analytes are loaded onto a C(8) column at 0.6 mL/min for 60s and eluted with a mixed eluent of 40% (v/v) 10 mmol/L sodium tetraborate buffer (pH 9.3) and 60% (v/v) ethanol at 0.75 mL/min. The MEKC separation is accomplished with a running buffer of 20 mmol/L sodium tetraborate (pH 9.3) containing 100 mmol/L sodium dodecyl sulfate (SDS) at 15 kV. For butyl p-hydroxybenzoate did not be detected in the cosmetic products, it was used as an internal standard (IS) added into the real samples. This FIA-SPE-MEKC method using IS allows the sample separation within 12 min and the sample throughput of five samples per hour with the relative standard deviation (R.S.D.) less than 2.3% (n=5). The limits of detection (LOD) are in the range from 0.07 to 0.1 microg/mL (S/N=3 and n=11). The proposed method has been used to determine three parabens in real cosmetic products satisfactorily.


Assuntos
Técnicas de Química Analítica/métodos , Cosméticos/química , Parabenos/análise , Técnicas de Química Analítica/normas , Cromatografia Capilar Eletrocinética Micelar , Análise de Injeção de Fluxo , Conservantes Farmacêuticos/análise , Extração em Fase Sólida
17.
J Chromatogr A ; 1171(1-2): 133-9, 2007 Nov 09.
Artigo em Inglês | MEDLINE | ID: mdl-17920070

RESUMO

A post-column reactor with coaxial-gap mode is developed for laser-induced fluorescence detection (LIF) in capillary electrophoresis (CE). The reactor can be assembled simply and conveniently, in which a thin polyimide sleeve of 10-mm length obtained from the capillary coating is used to align separation and reaction capillary with a 20 microm gap. Naphthalene-2,3-dicarboxaldehyde and 2-mercaptoethanol are used as derivatization reagents and delivered into the reaction capillary through the annulus between the separation capillary and polyimide sleeve and the gap of two capillaries by gravity. A reaction distance from the gap to detection point is 5mm. For the post-column reactor of CE-LIF, several configuration parameters are optimized, including liquid level difference between the derivatization solution and outlet buffer, annular dimension between the outer diameter of etched separation capillary and the inner diameter of polyimide sleeve, and reaction distance, etc. The detection limits in the range from 8.0x10(-8) to 1.0x10(-6) mol/L and linear calibration range more than two orders of magnitude are obtained for amino acids. The separation efficiency ranges from 1.35x10(5) to 1.67x10(5) theoretical plates.


Assuntos
Aminoácidos/análise , Técnicas de Química Analítica/métodos , Eletroforese Capilar/métodos , Lasers , Ácido Acético/análise , Técnicas de Química Analítica/instrumentação , Eletroforese Capilar/instrumentação , Análise de Injeção de Fluxo , Fluorescência , Sensibilidade e Especificidade
18.
Se Pu ; 25(2): 193-6, 2007 Mar.
Artigo em Chinês | MEDLINE | ID: mdl-17580684

RESUMO

An improved capillary electrophoretic (CE) separation and indirect ultraviolet (in-UV) detection system was proposed for the amino acid analysis in tea samples with a home-made partition cell and a background electrolyte (BGE) of p-aminobenzoic acid (PAB). PAB improved the separation efficiency and detection limits of the amino acids. The partition cell prevented PAB from chemical reaction at the electrode, reduced baseline noise and kept electric current inside the cell. The separation parameters of the amino acids, such as different BG-Es, BGE concentration, buffer pH and electroosmotic flow (EOF) modifiers, were investigated. The CE separation was carried out with the running buffer solution of pH 11. 2, 10 mmol/L PAB containing 0. 014 mmol/L cetyltrimethylamonium bromide (CTAB), an applied voltage of - 15 kV and a detection wavelength of 254 nm. Sixteen amino acids were separated within 14 min under the selected conditions. The linear ranges of the amino acids were 0. 02 - 0. 60 mmol/L except for theanine (0. 02 - 3. 80 mmol/L) and gamma-aminobutyric acid (0. 02 - 2. 00 mmol/L). The recoveries were in the range from 83. 0% to 106%. The relative standard deviations of peak area were less than 5% (n = 5) and the detection limits were in the range of 1. 7 -4. 5 gammamol/L. The method is fast, convenient and sensitive, and has been applied to the determination of 11 amino acids in tea samples satisfactorily.


Assuntos
Aminoácidos/análise , Eletroforese Capilar/métodos , Espectrofotometria Ultravioleta/métodos , Chá/química , Cetrimônio , Compostos de Cetrimônio/química , Concentração de Íons de Hidrogênio , Reprodutibilidade dos Testes
19.
Talanta ; 74(1): 1-6, 2007 Nov 15.
Artigo em Inglês | MEDLINE | ID: mdl-18371605

RESUMO

A simple and convenient method of micellar electrokinetic capillary chromatography (MEKC) using polyoxyethylene sorbitan monolaurate (Tween 20) to form single micelle and methanol as a buffer additive was introduced for the simultaneous determination of five polyphenols, including scopoletin, rutin, esculetin, chlorogenic acid and caffeic acid. A running buffer solution of pH 9.3, 20 mmol/L sodium tetraborate containing 64 mmol/L Tween 20 and 9% (v/v) methanol was adopted in the separation. Because rutin and esculetin were difficult to be separated by capillary zone electrophoresis (CZE) and SDS-based MEKC, Tween 20-based MEKC was adopted and the polyphenols were separated satisfactorily. The proposed method was used to determine the polyphenol components in the herbal medicine of Cortex fraxini. The separation mechanism of Tween 20-based MEKC for the polyphenols was discussed preliminarily.


Assuntos
Medicamentos de Ervas Chinesas/química , Flavonoides/análise , Fenóis/análise , Polissorbatos/química , Tensoativos/química , Aesculus , Cromatografia Capilar Eletrocinética Micelar , Flavonoides/química , Micelas , Fenóis/química , Polifenóis
20.
Se Pu ; 24(4): 392-5, 2006 Jul.
Artigo em Chinês | MEDLINE | ID: mdl-17017168

RESUMO

The separation of cigarette alkaloids was reported and performed with tartaric acid buffer solution by capillary zone electrophoresis (CZE). A buffer solution of pH 2.8, 410 mmol/L tartaric acid was used as the running buffer for the determination of cigarette alkaloids in CZE. The detection sensitivity and resolution with the tartaric acid buffer solution were better than those with phosphate buffer. The sample extraction conditions, buffer electrolyte, pH and concentrations were investigated for the alkaloids separation and determination. The linear range, detection limits, reproducibilities and recoveries of the cigarette alkaloids were 0.06 - 0.80 mg/L for nicotine (0.006 - 0.10 mg/L for other alkaloids), 0.002 - 0.01 mg/L, 2.2% - 10% and 87.6% - 102%, respectively.

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