Rapid detection of trace Hg~(2+) in animal matrix by specific DNA electrochemical sensor / 中国中药杂志

A highly specific electrochemical biosensor based on T-Hg~(2+)-T structure for fast screening trace Hg~(2+) in complex animal drug matrix was constructed by cyclic voltammetry(CV) and differential pulse voltammetry(DPV). In the presence of Hg~(2+), it can be specifically binded to the T base of DNA sequence on the surface of modified gold electrode, which changes the conformation of DNA molecule and the electrochemical signal. The concentration ratio of EDC/NHS, the concentration ratio of FC-DNA and the reaction time of the biosensor were optimized by the index of sensitivity and reproducibility in CV. The results showed that the stability of the biosensor was good within 3 days(RSD≤1.3%), the difference between batches was low(RSD=4.7%), and the specificity of the biosensor was high in the presence of interfering ions(As~(3+), Cd~(2+), Cu~(2+), Pb~(2+), Zn~(2+) and Fe~(3+)). DPV results showed that the peak current signal value has a linear relationship with the lgC_((Hg)) over a concentration range from 0.1 nmol·L~(-1) to 1.0 μmol·L~(-1) with a detection limit of 0.066 nmol·L~(-1). Finally, the recovery rate tested in the matrix of animal medicine was satisfactory as 99.17%-101.3%, which can meet the needs of the determination of trace Hg~(2+) in the matrix of Bombyx Batryticatus, and provide a new idea for the rapid screening of trace heavy metals in the matrix of other types of complex traditional Chinese medicine.

Determination of Phenol by an Electrochemical Method with Glassy Carbon Electrode / 中国药师

Objective: To establish an electrochemical method for the determination of phenol. Methods: An electrochemical workstation with three electrodes system was used with glassy carbon electrode as working electrode, Ag/AgCl as reference electrode and Pt as counter electrode. Cyclic voltammetry and differential pulse voltammetry were used for the determination of phenol. Results:Under the condition of 4% Na2SO4as the supporting electrolyte, phenol showed an obvious oxidation peak on the glassy carbon elec-trode. The peak current increased linearly with the concentration of phenol within the range of 0. 8 μg·ml-1-10. 2 μg·ml-1( r=0. 997 5). The lower limit of detection was 0. 20 μg·ml-1. The average recovery was 101. 2% (RSD=2. 2% , n=6). Conclusion:The method is simple and accurate, and can be used for the determination of phenol.

Differential pulse voltammetric determination of diclofenac in pharmaceutical preparations and human serum / Pulso diferencial determinação voltamétrica de diclofenaco em preparações farmacêuticas e em soro humano

This article describes a differential pulse voltammetric (DPV) method for the determination of diclofenac in pharmaceutical preparations and human serum. The proposed method was based on electro-oxidation of diclofenac at platinum electrode in 0.1 M TBAClO₄/acetonitrile solution. The well-defined two oxidation peaks were observed at 0.87 and 1.27 V, respectively. Calibration curves that obtained by using current values measured for second peak were linear over the concentration range of 1.5-17.5 μg mL^-1and 2-20 μg mL^-1 in supporting electrolyte and serum, respectively. Precision and accuracy were also checked in all media. Intra- and inter-day precision values for diclofenac were less than 3.87, and accuracy (relative error) was better than 4.12%. The method developed in this study is accurate, precise and can be easily applied to Diclomec, Dicloflam and Voltaren tablets as pharmaceutical preparation. In addition, the proposed technique was successfully applied to spiked human serum samples. No electro-active interferences from the endogenous substances were found in human serum...

Este artigo descreve um método de voltametria de pulso diferencial (VPD) para a determinação de diclofenaco em preparações farmacêuticas e em soro humano. O método proposto foi baseado em eletroxidação de diclofenaco no eléctrodo de platina em solução 0,1 M TBAClO₄/acetonitrila. Dois picos de oxidação bem definidos foram observados em 0,87 e 1,27 V, respectivamente. As curvas de calibração obtidas utilizando-se valores de corrente medidos por segundo pico foram lineares no intervalo de concentração de 1,5-17,5 μg mL^-1e 2-20 μg mL^-1em eletrólito suporte e soro, respectivamente. Precisão e exatidão também foram verificadas em todos os meios. Valores de precisão intra- e inter-dia para o diclofenaco foram inferiores a 3.87 e a precisão (erro relativo) foi melhor do que 4,12%. O método desenvolvido neste estudo é exato, preciso e pode ser facilmente aplicado a Diclomec, Dicloflam e comprimidos Voltaren, como preparação farmacêutica. Além disso, a técnica proposta foi aplicada com sucesso em amostras de soro humano. Não se observaram interferências das substâncias endógenas no soro humano...

Atividade antioxidante de extratos de folhas de ora-pro-nóbis (Pereskia aculeata Mill. ) usando métodos espectrofotométricos e voltamétricos in vitro / Antioxidant activity of ora-pro-nobis (Pereskia aculeata Mill. ) leaves extracts using spectrophotometric and voltammetric assays in vitro

Atualmente tem crescido a busca por plantas como fontes naturais de antioxidantes. Plantas com esta propriedade podem ser utilizadas para melhorar a qualidade de alimentos, seja para fins nutritivos ou de conservação, como também para a prevenção de doenças relacionadas ao aparecimento de radicais livres. A Pereskia aculeata Mill. (Ora-pro-nóbis) é uma espécie da família Cactaceae e suas folhas são consumidas por muitas pessoas. Neste contexto, este trabalho estudou o teor de fenóis totais (método Folin-Ciocalteau) e de proantocianidinas (vanilina sulfúrica), correlacionando-os com a atividade antioxidante (radical DPPH, sistema b-caroteno/ácido linoleico e voltametria por pulso diferencial) de extratos em acetona 80%, etanol 70% e água das folhas da espécie P. aculeata Mill., apresentando o extrato em acetona 80% maior teor de fenóis totais e proantocianidinas. Com relação à atividade antioxidante frente ao radical DPPH, o extrato em acetona 80% se apresentou ligeiramente melhor que o em etanol 70%. A técnica de voltametria por pulso diferencial mostrou que o extrato em acetona 80% apresenta constituintes com maior potencial redutor que o extrato em etanol 70%. Os dados obtidos a partir da voltametria corroboram com os resultados obtidos pelo método tradicional de DPPH. Os extratos em etanol 70% e em água apresentaram melhor atividade antioxidante pelo sistema b-caroteno/ácido linoleico, o que sugere a presença de outra classe de compostos que atuam na inibição do b- caroteno. Portanto, as folhas da espécie Pereskia aculeata podem ser consideradas como fonte potencial de compostos antioxidantes.

Currently, the search for plants as natural sources of antioxidants has been growing because they can be used to improve the nutritive or preservation properties of food, as soon as for the prevention of diseases related to free radicals. The Pereskiaaculeata Mill. (Ora-pro-nóbis,) is a specie of Cactaceae family and its leaves are consumed by many people. In this context, this paper studied the total phenols (Folin-Ciocalteu) and proanthocyanidins (vanillin sulfuric) correlating with the antioxidant activity (DPPH, b-carotene/linoleic acid system and differential pulse voltammetry) of extracts of 80% acetone, 70% ethanol and water of Pereskiaaculeata Mill. leaves. The 80% acetone extract showed higher total phenols and proanthocyanidins. Regarding to the antioxidant activity by DPPH radical scavenger, the 80% acetone extract was slightly better than 70% ethanol extract. The differential pulse voltammetry technique displayed that the 80% acetone extract presented constituents with greater reducing potential than the ones presented in 70% ethanol extract, what can corroborate the results obtained. The 70% ethanol and water extracts has shown better antioxidant activity by b-carotene/linoleic acid system, what probably suggests the presence of another compounds classes that are responsible for the inhibition the b-carotene. Therefore, the Pereskiaaculeata Mill. showed that its leaves may be considered as a potential source of antioxidant compounds.

Electrochemical Behavior and Determination of Pyridoxine Hydrochloride at Graphene-Carbon Nanotubes/Poly(nicotinic acid) Modified Electrode / 分析化学

Graphene ( GN) and multiwalled carbon nanotubes ( MWCNT) composites were coated on glassy carbon electrode ( GCE ) and then poly ( nicotinic acid ) ( PNA ) was electrodeposited on the modified electrode. The electrochemical behavior of pyridoxine hydrochloride ( VB6 ) was investigated at the modified electrode by cyclic voltammetry ( CV ) and differential pulse voltammetry ( DPV ) . Results showed the oxidation current of VB6 at the GN-MWCNT/PNA/GCE was obviously larger than that at GCE, PNA/GCE and GN/MWCNT/GCE. The oxidation process of VB6 was an irreversible diffusion-controlled process involving one electron and two protons. The liner range between the peak current intensity of DPV and the concentration of VB6 was 0 . 05-200 μmol/L with a detection limit of 0 . 02 μmol/L ( S/N=3 ) . The modified electrode showed a good reproducibility with a relative standard deviation of 3 . 1% ( n=8 ) . The proposed method was applied to the analysis of vitamin B6 in vitamin B6 tablets and compound vitamin B tablets with recoveries between 96 . 1%-104 . 5%.

Study on Electrochemical Behaviors and Determination of Xanthine and Uric Acid on Modified Glassy Carbon Electrode / 分析化学

The silver doped poly ( L-lysine ) modified glassy carbon electrode was fabricated by cyclic voltammetry, the surface of the electrode was characterized by scanning electron microscopy and electrochemical impedance spectroscopy. The electrochemical behaviors and the simultaneous detection of xanthine and uric acid were studied by cyclic voltammetry and differential pulse voltammetry. The results indicated that this modified electrode exhibited excellent electrocatalytic activity towards the oxidation of xanthine and uric acid. The stable oxidation peaks of xanthine and uric acid appeared with the peak potential of 0. 980V and 0. 600V respectively at the modified electrode in pH 3. 0 phosphate buffer solution. The oxidation peaks of xanthine and uric acid were separated at 380 mV. Under the optimum conditions, the linear ranges for the determination of xanthine and uric acid were 1 . 00 × 10-6-2 . 50 × 10-4 mol/L respectively by differential pulse voltammetry. The detection limits were 5. 0×10-7mol/L. The method has been applied to the simultaneous detection of xanthine and uric acid in healthy human urine with satisfactory results.

Development and validation of an electroanalytical methodology for determination of isoniazid and rifampicin content in pharmaceutical formulations / Desenvolvimento e validação de uma metodologia eletroanalítica para a determinação do teor de isoniazida e rifampicina em preparações farmacêuticas

Tuberculosis remains a major public health problem, especially in developing countries. Brazil presents the largest number of cases in Latin America and is among the 22 countries considered priorities by the World Health Organization (WHO). The Rio de Janeiro state has the largest number of cases registered in the country. The treatment of patients, commonly, makes use of the drugs isoniazid and rifampicin for six months. This study aimed to develop and validate an electroanalytical methodology, using the technique of differential pulse voltammetry for the determination of these drugs in the associated form, in order to evaluate the quality of medicines distributed in the state of Rio de Janeiro. The potential reduction for the isoniazid and rifampicin were -1.10 and -0.90 V. The developed and validated electroanalytical method presented a linear range of 0.25 to 1.25 mg/L to isoniazid, limits of detection and quantification of 0.05 and 0.14 mg/L, and recovery of 98.2 ± 0.4 percent; a tracking linear of 0.40 to 2.00 mg/L for rifampicin, with limits of detection and quantification of 0.07 and 0.19 mg/L and recovery of 95.8 ± 0.6 percent. Six lots of medicines from two pharmaceutical companies were analyzed. Only one of the samples showed unsatisfactory levels of rifampicin.

A tuberculose continua sendo um importante problema de saúde pública, especialmente em países em desenvolvimento. O Brasil apresenta o maior número de casos da América Latina, estando entre os 22 países considerados prioritários nas ações de controle da doença pela Organização Mundial da Saúde (OMS). No Brasil, o Rio de Janeiro é o estado com o maior número de casos registrados no país. O tratamento de doentes com tuberculose faz uso dos fármacos isoniazida e rifampicina durante seis meses. O presente trabalho objetivou desenvolver e validar metodologia eletroanalítica, utilizando a técnica de voltametria de pulso diferencial, para a determinação desses dois princípios ativos na forma associada e avaliar a qualidade dos medicamentos distribuídos no estado do Rio de Janeiro. Os potenciais de redução para a isoniazida e rifampicina foram respectivamente -1,10 e -0,90 V. O método eletroanalítico desenvolvido e validado apresentou para a isoniazida faixa linear de 0,25 a 1,25 mg/L, limites de detecção e quantificação de 0,05 e 0,14 mg/L e recuperação de 98,2 ± 0,4 por cento; para a rifampicina faixa linear de 0,40 a 2,00 mg/L, limites de detecção e quantificação de 0,07 e 0,19 mg/L e recuperação de 95,8 ± 0,6 por cento. Foram analisados 6 lotes de medicamentos de dois laboratórios farmacêuticos. Apenas uma das amostras apresentou teor de rifampicina insatisfatório.