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1.
Artigo em Inglês | MEDLINE | ID: mdl-27805474

RESUMO

A fast, inexpensive and sensitive approach for the simultaneous determination of chlortetracycline, ampicilline and sarafloxacin in milk was developed using capillary electrophoresis coupled with an electrochemiluminescence detector. Under the optimal detection conditions, the linear ranges for chlortetracyline, ampicilline and sarafloxacin were 0.030-5.0, 0.050-5.0 and 0.0040-2.0 µg ml-1, respectively. The correlation coefficients of chlortetracycline, ampicilline and sarafloxacin were determined as 0.9997, 0.9952 and 0.9978, respectively. Detection limits (S/N = 3) of chlortetracycline, ampicilline and sarafloxacin were found as 0.017, 0.018 and 0.0013 µg ml-1, respectively. This method was successfully applied for the determination of chlortetracycline, ampicilline and sarafloxacin in milk. The recoveries were between 95.3% and 100%. The relative standard deviations of the detection limit and recovery were less than 2.6% and 3.2%, respectively.


Assuntos
Ampicilina/análise , Clortetraciclina/análise , Ciprofloxacina/análogos & derivados , Eletroforese Capilar/métodos , Leite/química , Animais , Ciprofloxacina/análise , Técnicas Eletroquímicas/métodos , Limite de Detecção , Medições Luminescentes , Reprodutibilidade dos Testes
2.
Artigo em Inglês | MEDLINE | ID: mdl-26551206

RESUMO

A simple, sensitive and selective method for determination of urapidil hydrochloride was developed using capillary electrophoresis with electrochemiluminescence (CE-ECL) technique for the first time. Under the optimized experimental conditions, the ECL intensity was linear with the concentration of urapidil hydrochloride in the range from 0.050 to 50.0ng/mL and the detection limit was 0.014ng/mL (S/N=3). The proposed method was used for studying pharmacokinetics of urapidil hydrochloride in rat plasma and the main pharmacokinetic parameters of the peak concentration (Cmax), half life time (T1/2) and peak concentration time (Tmax) were 240.45±21.15ng/mL, 0.58±0.16h and 1.08±0.13h, respectively. The recoveries of urapidil hydrochloride in the diluted extracts of rat plasma samples ranged from 96.68 to 98.82%. The RSD was lower than 3%.


Assuntos
Eletroforese Capilar/métodos , Medições Luminescentes/métodos , Piperazinas/sangue , Piperazinas/farmacocinética , 2,2'-Dipiridil/análogos & derivados , Animais , Limite de Detecção , Modelos Lineares , Compostos Organometálicos , Piperazinas/química , Ratos , Reprodutibilidade dos Testes
3.
J Chromatogr A ; 1395: 173-9, 2015 May 22.
Artigo em Inglês | MEDLINE | ID: mdl-25865795

RESUMO

A new method for selenium speciation in fermented bean curd wastewater and juice was described. This method involved sample extraction with 5-sulfosalicylic acid (SSA)-functionalized silica-coated magnetic nanoparticles (SMNPs), capillary electrophoresis (CE) separation, and online detection with a modified electrothermal atomic absorption spectrometry (ETAAS) system. The modified interface for ETAAS allowed for the introduction of CE effluent directly through the end of the graphite tube. Elimination of the upper injection hole of the graphite tube reduced the loss of the anlayte and enhanced the detection sensitivity. The SSA-SMNPs were synthesized and used to extract trace amounts of selenite [Se(IV)], selenite [Se(VI)], selenomethionine (SeMet), and selenocystine (SeCys2) from dilute samples. The concentration enrichment factors for Se(VI), Se(IV), SeMet, and SeCys2 were 21, 29, 18, and 12, respectively, using the SSA-SMNPs extraction. The limits of detection for Se(VI), Se(IV), SeMet, and SeCys2 were 0.18, 0.17, 0.54, 0.49ngmL(-1), respectively. The RSD values (n=6) of method for intraday were observed between 0.7% and 2.9%. The RSD values of method for interday were less than 3.5%. The linear range of Se(VI) and Se(IV) were in the range of 0.5-200ngmL(-1), and the linear ranges of SeMet and SeCys2 were 2-500 and 2-1000ngmL(-1), respectively. The detection limits of this method were improved by 10 times due to the enrichment by the SSA-SMNP extraction. The contents of Se(VI) and Se(IV) in fermented bean curd wastewater were measured as 3.83 and 2.62ngmL(-1), respectively. The contents of Se(VI), Se(IV), SeMet, and SeCys2 in fermented bean curd juice were determined as 6.39, 4.08, 2.77, and 4.00ngmL(-1), respectively. The recoveries were in the range of 99.14-104.5% and the RSDs (n=6) of recoveries between 0.82% and 3.5%.


Assuntos
Benzenossulfonatos/química , Técnicas de Química Analítica/métodos , Eletroforese Capilar , Nanopartículas de Magnetita/química , Salicilatos/química , Selênio/química , Espectrofotometria Atômica , Limite de Detecção , Selênio/isolamento & purificação , Dióxido de Silício/química , Águas Residuárias/química
4.
Anal Chim Acta ; 851: 37-42, 2014 Dec 03.
Artigo em Inglês | MEDLINE | ID: mdl-25440662

RESUMO

The paper describes a homemade ultrasonic microdialysis device coupled with capillary electrophoresis electrochemiluminescence (CE-ECL) for studying the interaction between human serum albumin (HSA) and trimetazidine dihydrochloride (TMZ). The time required for equilibrium by ultrasonic microdialysis was 45min, which was far less than that by traditional dialysis (240min). It took 80min to achieve the required combination equilibrium by normal incubation and only 20min by ultrasonic. Compared with traditional dialysis, the use of ultrasonic microdialysis simplified experimental procedures, shortened experimental time and saved consumption of sample. A simple, sensitive and selective determination of TMZ was developed using CE-ECL and the parameters that affected ECL intensity were optimized. Under the optimized conditions, the linear range of TMZ was from 0.075 to 80µmol/L (r(2)=0.9974). The detection limit was 26nmol/L with RSD of 2.8%. The number of binding sites and binding constant were 1.54 and 15.17L/mol, respectively.


Assuntos
Eletroforese Capilar/métodos , Medições Luminescentes/métodos , Microdiálise/métodos , Albumina Sérica/metabolismo , Trimetazidina/metabolismo , Ultrassom , Sítios de Ligação , Soluções Tampão , Eletroquímica , Humanos , Concentração de Íons de Hidrogênio , Limite de Detecção , Modelos Lineares , Ligação Proteica , Reprodutibilidade dos Testes , Albumina Sérica/química , Integração de Sistemas , Fatores de Tempo , Trimetazidina/química
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