Determination of Entacapone by Differential Pulse Polarography in Pharmaceutical Formulation

Abstract

The electrochemical methods, sampled direct current, and differential pulse polarography, were developed successfully and applied to the routine determination of Entacapone in pharmaceutical formulation. Both methods gave rise to three reduction waves or peaks respectively. The irreversibility and the diffusion‐controlled of the first reduction were confirmed by cyclic voltammetry. The limiting currents are directly proportional to the concentration of entacapone with a correlation coefficient of 0.99. The within‐day coefficients of variation and the day‐to‐day coefficient of variation were less than 3.5% for entacapone and Comtan^®. The percentage recovery for entacapone in tablets is satisfactory for both methods. The method is simple without any pretreatment.     

The Determination of Nitrite and Nitrate Ions by Differential Pulse Polarography

Abstract

A previously reported method for the determination of nitrite ion has been extended to include nitrate ion. Nitrate is reduced to nitrite by a cadmium column and the nitrite ion determined as diphenylnitrosamine. Cadmium interference is removed by pH adjustment and the use of KDTA.     

Simultaneous Trace Determination of Nickel and Cobalt in Natural Waters by Differential Pulse Polarography

Abstract

A differential pulse polarographic method has been developed for the simultaneous low level determination of nickel and cobalt in the presence of furildioxime in natural waters. The nature of the electrode processes was studied with cyclic voltammetry. Limits of determination of 0.4 μg/L and 0.15 μg/L were achieved for nickel and cobalt respectively     

磺胺甲恶唑的二阶导数差示脉冲极谱法测定

建立了磺胺甲恶唑的二阶导数差示脉冲极谱定量分析方法,磺胺甲恶唑在１０％ＨＣｌ－（硼酸－氯化钾缓冲溶液）－水（５：５：９０）的底液中,于－１．４５Ｖ（ｖｓ．Ａｇ／ＡｇＣｌ）处出现一良好的二阶导数差示脉冲极谱峰,磺胺甲恶唑浓度与其峰高在０．０８～０．８０ｍｍｏｌ／Ｌ范围内呈线性关系（ｐ〈０．０１）,检测限为８．６ｎｍｏｌ／Ｌ。本法简便、快速、灵敏、结果准确。     

一阶导数差示脉冲极谱法用于甲硝唑的定量研究

本实验运用一阶导数差示脉冲极谱法对甲硝唑及其制剂进行了定量研究。在０．００１ｍｏｌ／Ｌ氯化钾－０．００１ｍｏｌ／Ｌ盐酸－水（１＋０．２＋４８）的底液中，甲硝唑于－０．８００Ｖ（ｖｓ Ａｇ／ＡｇＣｌ）处出现一良好的一阶导数差示脉冲极谱峰，在５０～３００μｇ／ｍＬ范围内，药物浓度与其导数峰幅值呈线关系，检测限为８．０×１０＾－８ｍｏｌ／Ｌ。本法操作简便，快速，灵敏，结果准确。     

Rapid Differential Pulse Polarographic Determination of Thiamethoxam in Commercial Formulations and some Real Samples

The polarographic behavior of thiamethoxam (a neonicotinoid insecticide) was studied by direct current and differential pulse polarography. Depending on the pH thiamethoxam exhibited one or two well-defined cathodic polarographic waves. The characteristics of the electrode reaction were investigated and it was found that at pH > 5.0 the target molecule captures four electrons in the first step, and two in the second. Based on the reduction behavior of the target molecule on the mercury electrode, a differential pulse polarographic method was elaborated for the rapid determination of thiamethoxam at pH 8.0. With the optimized method, a linear response for thiamethoxam was found in the concentration range of 31.1 − 470 ng cm⁻³, the relative standard deviation did not exceed 1.6%, and the detection and quantitation limits were found to be 9.3 ng cm⁻³ and 31.1 ng cm⁻³, respectively. The method was applied to the determination of thiamethoxam in commercial formulations and real samples (potato and maize). The procedure is simple, fast, sensitive, and compares well with comparative spectrophotometric and chromatographic (HPLC/DAD) methods.     

Determination of Benzoylmetronidazole in Suspension Formulations by Differential Pulse Polarography

Abstract

A rapid, reproducible and accurate method for the determination of benzoylmetronidazole in pharmaceutical suspensions is presented. Differential pulse polarography at a static mercury drop electrode is used for the reduction of the nitro group of benzoylmetronidazole.     

Determination of Chloramphenicol (CAP) in Food Products by Differential Pulse Polarography

ABSTRACT

The electrochemical determination of chloramphenicol (CAP) in food using mini- and micro- mercury drop electrodes and differential pulse polarography (DPP) has been elaborated. A phosphate buffer with pH 6.6 was used as the basic electrolyte. The analysis was based on a peak at the potential E_p = ?0.320 V which showed a clearly linear dependence of the peak current on the concentration of chloramphenicol in the sample under investigation. Prior to the determination of chloramphenicol in actual samples it was necessary to extract this antibiotic with organic solvents such as methanol, ethanol and ethyl acetate.

In order to separate CAP in its basic form, various modifications of sample preparation procedures were made for the analysis with the use of selected hydrolytic enzymes. The determined quantities of CAP in the samples of meat, milk, eggs and their products ranged in the ng/g d.w. range.

For purposes of comparison and verification of the electrochemical results of CAP determination, chloramphenicol was determined in the same samples, by the immunoenzymatic method ELISA.     

一阶导数差示脉冲极谱法用于扑热息痛的定量分析

一阶导数差示脉冲极谱法用于扑热息痛及其制剂的定量分析，在乙醇－水－２．０×１０＾－＾３ｍｏｌ／ＬＨ２ＳＯ４（１２．５：１１．５：１）的溶液中，于０．２４Ｖ（ｕｓＡｇ／ＡｇＣｌ）处出现良好的一阶导数差示脉冲极谱峰，在３．３×１０＾－＾４～３．３×１０＾－＾３ｍｏｌ／Ｌ范围内，浓度与其一阶导数差示脉冲极谱峰值呈线性关系，检测限为７．８×１０＾－＾８ｍｏｌ／Ｌ。方法简便，快速，灵敏，结果准确。     

磺胺二甲嘧啶钠的二阶导数差示脉冲极谱法定量研究

建立了磺酸二甲嘧啶钠的二阶导数差示脉冲极谱定量分析方法,磺胺二甲嘧啶钠在乙醇－（硼酸－氯化钾缓冲液）－水（体积比７０：２：２８）的底液中,于－１．５６０Ｖ（ｖｓ．Ａｇ／ＡｇＣｌ）处出现一良好的二阶导数差示脉冲极谱峰,磺胺二甲嘧啶钠浓度与其峰幅值在０．０６～０．６ｍｍｏｌ．Ｌ＾－１范围内呈非常显著的线性关系（Ｐ〈０．０１）,检出限为９．２ｎｍｏｌ．Ｌ＾－１,已用于注射液中磺酸二甲嘧啶钠的测定。     

微分脉冲极谱同时测定三种碱性氨基酸的研究

应用微分脉冲极谱，在ｐＨ９．０ ＮａＢ４Ｏ７－ ＣＨ３ＣＨＯ－Ｃｏ２＋－ ＮａＯＨ组成的极谱底液，扫描电位－ ０．８０～－ １．６０ Ｖ、振幅 ２０ｍＶ、扫描速度５ｍＶ／ｓ、一滴汞周期２ｓ的条件下进行连续扫描测量三种碱性氨基酸，获得三个灵敏 度和分辨率均较高的极谱峰图。该法简便快速，稳定可靠，为测量各种蛋白质中的三种磁性氨基酸提供一种新途 径。     

Determination of Codeine,Dionin and Thebaine by Differential Pulse Polarography

Abstract

The method proposed for determining codeine, dionin and thebaine by differential pulse polarography is based on the reduction (in ammoniacal medium) of the nitroderivatives obtained by dissolving the substances in concentrated nitric acid. The values of the reduction potentials range between -0.45 and -0.69 V. Morphine and heroine do not interfere in the determination of the mentioned alkaloids.     

维生素C及其制剂的一阶导数差示脉冲极谱法测定

本文建立了维生素Ｃ及其制剂的一阶导数差示脉冲极谱定量分析方法，在水溶液中，维生素Ｃ于－１．１０Ｖ（ｖｓＡｇ／ＡｇＣｌ）处出现一良好的一阶导数差示脉冲极谱峰，在１～１７５μｇ／ｍＬ范围内，维生素Ｃ浓度与其一阶导数差示脉冲极谱峰幅值呈非常显著的线性关系（Ｐ〈０．０１），方法简便，快速，灵敏，结果准确。     

定量测定秦皮中秦皮甲素的二阶导数示差脉冲极谱法

建立了中草药秦皮中秦皮甲素的二阶导数示差脉冲极谱定量分析方法。秦皮甲素在乙醇－2mol/L氯化锂－水（体积比2：1：5）的底液中,于－1．703V（vs Ag/AgCl)处出现一良好的二阶导数示差脉冲极谱峰,其峰幅值与秦皮甲素在0．2－1．6mmol/L范围内呈非常显著的线性关系（P＜0．01）,检测下限脒50mmol/L。该法简便、快速、灵敏,结果准确。     

Differential Pulse Polarographic Determination of Orthophosphate in Nonaqueous Media

Abstract

The method is based on the polarographic behavior of 12-tungstophosphoric acid in nonaqueous media at the DME utilizing the differential pulse polarographic technique. In this procedure, orthophosphate is converted to 12-tungstophosphoric acid H₃ PW ₁₂ O ₄₀ by reacting with tungstate under acidic conditions and at 100°C. The H₃ PW ₁₂ O ₄₀ is extracted into 1-pentanol and its polarographic measurement is made in 1-pentanol-ethanoi mixture containing sodium perchlorate as supporting electrolyte. The differential pulse polarogram of H₃ PW ₁₂ O ₄₀ in this solution shows three peaks between 0.00 and -0.90 V vs. Ag/ AgCl. The most cathodic peak at -0.78 V exhibited the highest peak current value and was used for the analytical measurement. A linear calibration graph in the range 0.10 - 5.00 pg/ml P in the final solution was obtained. The method has a relative standard deviation of 0.90% at the 4 pg/ml P level and 1.32% at the 1 μg/ml P level in the final solution. Arsenate, borate and silicate do not interfere.     

有机锗(锗-132)的示差脉冲极谱研究

用示差脉冲极谱法,在pH1.30H_2SO_4和3,4-二羟基苯甲醛(DHB)底液中,获得了有机锗(Ge-132)和无机锗Ge(Ⅳ)二个配位吸附极谱波,波峰分别为E_P2-0.62V和E_pl=-0.47V(υs.AgCI/Ag),Ge-132浓度在2.6×10_(-5)～3.1×10_（-3）mol/L范围内,Ge(Ⅳ)浓度在 3.1×10_（-5）～2.1×10_（-4）mol/L范围内分别与峰电流星线性关系.利用该示差脉冲极谱法可同时测定Ge-132和Ge(Ⅳ),用于有机锗营养口服液中Ge-132和Ge(Ⅳ)的测定结果满意.还探讨了Ge-132极谱波的性质,测定了有关动力学参数.     

极谱法测定蒙药那如三味丸中锗的研究

采用差分脉冲极谱法,在pH 1.50、含3,4 –二羟基苯甲醛(DHB)的H2SO4中,测得无机锗的峰电位为Ep=-0.54 V,Ge(Ⅳ)浓度在1.04×10 5～1.05×10 4 mol·L 1范围内与峰电流呈线性关系,利用该法用于测定蒙药那如三味丸中总锗、无机锗和有机锗,得到了满意的结果.     

Determination of Germanium in Zinc by Differential Cathode Ray Polarography

Abstract

A differential cathode ray polarographic method is described for determining traces of germanium in zinc and its compounds. The germanium was previously extracted with carbon tetrachloride from the sample solution in hydrochloric acid. After reextraction with water the germanium content was determined polarographically in 1.4 M perchloric acid ? 5.10^?2 M pyrogallol. The detection limit was 0.0012 μg/ml, allowing to detect about 4 ppb of germanium in zinc using 5 g samples.     

两种蒙药中锗的差示脉冲极谱测定及其红外光谱的差异

采用差示脉冲极谱法,以3,4-二羟基苯甲醛的0.072 mol·L-1硫酸溶液作为底液,在峰电位为-0.53 Ⅴ(vs．Ag/AgCl),锗(Ⅳ)浓度在1.03×10-5～1004×10-4mol·L-1范围内与峰电流呈线性关系.据此测定了阿嘎日-35和阿嘎日-8中总锗、无机锗、有机锗含量,并利用红外光谱比较了两种蒙药的红外谱图的差异,据此可对两种蒙药予以区别.