“…8,[21][22][23] The response obtained by square-wave voltammetry is dependent on parameters such as frequency (f), pulse height (DE p ) and scan increment (DE s ), which have a combined influence on the peak current. Hence, they were analyzed in order to optimize the experimental set-up for sulfadiazine determination.…”
Section: Optimization Of Square-wave Voltammetry Parametersmentioning
Sulfadiazina foi quantificada em duas amostras de produtos farmacêuticos usando voltametria de onda quadrada. O sinal analítico foi obtido por redução em vez de oxidação da sulfa sobre eletrodo de carbono vítreo. A determinação eletroanalítica foi realizada em solução-tampão Britton-Robinson 0,04 mol L -1 com pH 6,8. A redução irreversível da sulfadiazina foi observada em -1,49 V vs. Ag/AgCl. A curva analítica foi obtida na faixa de concentração entre 62,7 e 340 µmol L -1 (r = 0,9986) e o limite de detecção foi 10,9 µmol L -1. Para uma amostra analisada, os valores de recuperação ficaram entre 94,9 e 101,1%, enquanto para a outra amostra foram entre 96,0 e 104,6%, indicando que a composição da matriz não interfere nos resultados analíticos. A exatidão do método eletroanalítico foi comparada com o método padrão de titulação amperométrica.Sulfadiazine was quantified in two samples of pharmaceutical preparations by square-wave voltammetry. The analytical signal response was obtained by electrochemical reduction instead of oxidation of the sulfa drug at a glassy carbon electrode. The determination was carried out in 0.04 mol L -1 Britton-Robinson pH 6.8 buffer solution. Sulfadiazine reduction was observed at -1.49 V vs. Ag/AgCl in one well-resolved irreversible peak. The analytical curve was obtained in the concentration range of 62.7 to 340 µmol L -1 (r = 0.9986) with a detection limit of 10.9 µmol L -1 . For one sample analyzed, recovery values were in the range of 94.9 to 101.1%, while for the other sample they were within 96.0 to 104.6%, indicating no matrix interference effects on the analytical results for both sulfadiazine samples. The accuracy of the electroanalytical method was compared to the standard amperometric titration method.
“…8,[21][22][23] The response obtained by square-wave voltammetry is dependent on parameters such as frequency (f), pulse height (DE p ) and scan increment (DE s ), which have a combined influence on the peak current. Hence, they were analyzed in order to optimize the experimental set-up for sulfadiazine determination.…”
Section: Optimization Of Square-wave Voltammetry Parametersmentioning
Sulfadiazina foi quantificada em duas amostras de produtos farmacêuticos usando voltametria de onda quadrada. O sinal analítico foi obtido por redução em vez de oxidação da sulfa sobre eletrodo de carbono vítreo. A determinação eletroanalítica foi realizada em solução-tampão Britton-Robinson 0,04 mol L -1 com pH 6,8. A redução irreversível da sulfadiazina foi observada em -1,49 V vs. Ag/AgCl. A curva analítica foi obtida na faixa de concentração entre 62,7 e 340 µmol L -1 (r = 0,9986) e o limite de detecção foi 10,9 µmol L -1. Para uma amostra analisada, os valores de recuperação ficaram entre 94,9 e 101,1%, enquanto para a outra amostra foram entre 96,0 e 104,6%, indicando que a composição da matriz não interfere nos resultados analíticos. A exatidão do método eletroanalítico foi comparada com o método padrão de titulação amperométrica.Sulfadiazine was quantified in two samples of pharmaceutical preparations by square-wave voltammetry. The analytical signal response was obtained by electrochemical reduction instead of oxidation of the sulfa drug at a glassy carbon electrode. The determination was carried out in 0.04 mol L -1 Britton-Robinson pH 6.8 buffer solution. Sulfadiazine reduction was observed at -1.49 V vs. Ag/AgCl in one well-resolved irreversible peak. The analytical curve was obtained in the concentration range of 62.7 to 340 µmol L -1 (r = 0.9986) with a detection limit of 10.9 µmol L -1 . For one sample analyzed, recovery values were in the range of 94.9 to 101.1%, while for the other sample they were within 96.0 to 104.6%, indicating no matrix interference effects on the analytical results for both sulfadiazine samples. The accuracy of the electroanalytical method was compared to the standard amperometric titration method.
“…Furthermore, the detection limit of the proposed method (0.8 µg/L) is lower than the previously reported methods. [5][6]10,12,15,[17][18][19][20] The main advantages of the method are simplicity, rejection of matrix constituents, high sensitivity, low cost, speed of analysis and applicability for various real samples (tablet, milk and urine samples). …”
Section: Conculsionmentioning
confidence: 99%
“…Several analytical procedures for the determination of sulfadiazine have been reported in the literature. Among them are reversed phase high performance liquid chromatography coupled with on-line atmospheric pressure chemical ionization mass spectrometry (HPLC/APCI-MS), 4 capillary zone electrophoresis, 5 18 and FIA system with amperometric detection. 19 However, most of them either require complicated and ex-pensive instruments, 4,[8][9][10][11]15,16 or are time consuming, 4,6,[12][13][14] or have high detection limit.…”
Section: Introductionmentioning
confidence: 99%
“…19 However, most of them either require complicated and ex-pensive instruments, 4,[8][9][10][11]15,16 or are time consuming, 4,6,[12][13][14] or have high detection limit. 5,7,8,14,15,18 Therefore, the need for a sensitive, simple and reliable method for the determination of sulfadiazine is well recognized. Flame atomic absorption spectroscopy is a versatile, simple and high speed instrument for direct determination of metal ions, [20][21][22][23][24][25] but its use in indirect determination of nonmetallic anions and drugs is limited.…”
An indirect simple and rapid cloud point extraction is proposed for separation and preconcentration of sulfadiazine and its determination by flow injection-flame atomic absorption spectroscopy (FI-FAAS). The sulfadiazine from 35 mL of solution was readily converted to silver sulfadiazine upon addition of silver nitrate (9.7 × 10 -5 mol/L). Then, Triton X-114 a non ionic surfactant was added and the solution was heated to 60°C. At this stage, two separate phases was formed and silver sulfadiazine enters the surfactant rich phase of non-ionic micelles of Triton X-114. The surfactant-rich phase (~50 µL) was then separated and diluted to 300 µL with acidic methanol. The concentration of silver in the surfactant-rich phase which is proportional to the concentration of sulfadiazine in sample solution was determined by FI-FAAS. The parameters affecting extraction and separation were optimized. Under the optimum conditions (i.e. pH 2-10, silver concentration (9.7 × 10 -5 mol/L), Triton X-114 (0.075% v/v) and temperature 60°C) a preconcentration factor of 117 and a relative standard deviation of 4.9% at 37 mg L -1 of sulfadiazine was obtained. The method was successfully applied to analysis of milk, urine and tablet samples and accuracy was determined by recovery experiments.
“…1) is one of these sulphonamide antibiotics used in freshwater aquaculture. It has been routinely determined by conventional optical and electrical methods [10,11], HPLC-based procedures [12] and ELISA [13] but a single method that could lead to a low cost procedure with limits of detection capable of on-site application in aquaculture waters has never been envisaged.…”
A B S T R A C TSulfadimethoxine (SDM) is one of the drugs, often used in the aquaculture sector to prevent the spread of disease in freshwater fish aquaculture. Its spread through the soil and surface water can contribute to an increase in bacterial resistance. It is therefore important to control this product in the environment. This work proposes a simple and low-cost potentiometric device to monitor the levels of SDM in aquaculture waters, thus avoiding its unnecessary release throughout the environment. The device combines a micro-pipette tip with a PVC membrane selective to SDM, prepared from an appropriate cocktail, and an inner reference solution. The membrane includes 1% of a porphyrin derivative acting as ionophore and a small amount of a lipophilic cationic additive (corresponding to 0.2% in molar ratio). The composition of the inner solution was optimized with regard to the kind and/or concentration of primary ion, chelating agent and/or a specific interfering charged species, in different concentration ranges. Electrodes con-structed with inner reference solutions of 1 x 10 -8 mol/L SDM and 1 x 10 -4 mol/L chromate ion showed the best analytical features. Near-Nernstian response was obtained with slopes of -54.1 mV/decade, an extraordinary detection limit of 7.5 ng/mL (2.4 x 10 -8 mol/L) when compared with other electrodes of the same type. The reproducibility, stability and response time are good and even better than those obtained by liquid contact ISEs.Recovery values of 98.9% were obtained from the analysis of aquaculture water samples.
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