塞曲司特的吸附伏安法测定

目的建立吸附伏安法测定塞曲司特。方法在0.3mol/LKH2PO4-Na2HPO4(pH6.40)底液中,塞曲司特在汞电极上有一线性扫描还原峰,峰电位Ep=-1.16 V(vsAg/AgCl),该峰具有明显的吸附性。结果吸附粒子为塞曲司特中性分子,建立了吸附溶出伏安法测定塞曲司特的最佳条件,方法的检出限为2×10-8mol.L-1。结论方法灵敏度高,重现性好,结果准确。     

A novel chemiluminescence method for determination of terbutaline sulfate based on potassium ferricyanide oxidation sensitized by rhodamine 6G

This work reports a novel flow injection-chemiluminescence (FI-CL) system for determination of terbutaline sulfate, a drug for treatment of asthma and chronic obstructive pulmonary disease (COPD). It is based on the reaction of potassium ferricyanide with terbutaline sulfate in sodium hydroxide medium sensitized by the fluorescent dye rhodamine 6G. With the peak height as a quantitative parameter applying optimum working conditions, terbutaline sulfate is determined over the range of 0.01-1.2 microg ml(-1) with a detection limit of 6.7 x 10(-3) microg ml(-1). The relative standard deviation (R.S.D.) is 3.7% for 0.1 microg ml(-1) terbutaline sulfate (n = 11). The proposed method is sensitive, simple, rapid, and was applied to determination of terbutaline sulfate in pharmaceutical preparations. The possible chemiluminescence (CL) reaction mechanism was also discussed briefly.     

Determination of cadmium by differential pulse adsorptive stripping voltammetry

A study of the adsorptive stripping voltammetry of cadmium on a mercury drop electrode is reported in which 2-mercapto-5-phenyl-amino-1,3,4-thiadiazole (MPATD), synthesized at home has been used as a chelating agent. The most suitable operating conditions and parameters such as buffer, pH, deposition potential, deposition time, ligand concentration, scan rate and others were selected and the determination of cadmium from aqueous solutions using the standard additions method was possible. As validation criteria, the linearity and range, repeatability of the signal, repeatability of the concentration and accuracy were investigated. A limit of detection of 4.67 x 10(-10) M and a limit of quantification of 1.55 x 10(-9) M were achieved. The interference of other metals and organic substances was studied. Concerning a possible catalytic effect, no one was found. The method was designed in order to determine Cd from biological samples.     

Determination of Norfloxacin by square-wave adsorptive voltammetry on a glassy carbon electrode

The adsorptive and electrochemical behavior of norfloxacin on a glassy carbon electrode were investigated by cyclic and square-wave voltammetry. Cyclic voltammetric studies indicated that the process was irreversible and fundamentally controlled by adsorption. To obtain a good sensitivity, the solution conditions and instrumental parameters were studied using square-wave voltammetry. In acetate buffer of pH 5.0, norfloxacin gave a sensitive adsorptive oxidative peak at 0.920 V (versus Ag-AgCl). Applicability to measurement of norfloxacin at submicromolar levels in urine samples was illustrated. The peak current was linear with the norfloxacin concentration in the range 5-50 microg ml(-1) urine. The detection limit was 1.1 microg ml(-1) urine.     

Determination of melatonin in galenic preparations by LC and voltammetry

The amount of melatonin in galenic tablets was determined by means of two feasible and accurate analytical methods. The high performance liquid chromatography (HPLC) with ultraviolet detection at 223 nm used a C(18) reversed-phase column; the linear scan voltammetric procedure (LSV) employs a pH 3.0 phosphate buffer as the supporting electrolyte for the oxidation process of melatonin, which has a current intensity maximum at +850 mV. The two methods gave satisfactory results in terms of precision and accuracy. In fact, the data of repeatability and intermediate precision expressed as percentage relative standard deviations (RSD%) were < or =2.8 and the accuracy values, resulting from recovery experiments, were between 99.0 and 101.3%. Both methods are suitable for quality control of melatonin in galenic preparations; the LSV procedure is more rapid, the HPLC method is more sensitive and more precise.     

差示脉冲伏安法测定中药秦皮中秦皮乙素的含量

目的:研究秦皮乙素在碳糊电极(CPE)上的伏安行为,建立中药秦皮中秦皮乙素含量测定的新方法。方法:采用循环伏安法研究秦皮乙素在电极上的电化学行为,以差示脉冲伏安对其含量进行测定。结果:在pH4.0磷酸缓冲液中,氧化峰电流与秦皮乙素浓度在5.0×10-7~4.5×10-6mol·L-1范围内呈良好的线性关系,检测限为6.0×10-8mol·L-1。结论:CPE可有效消除样品中其他组分对秦皮乙素测定的干扰,已成功用于实际样品中秦皮乙素含量的测定。该方法灵敏度高、检测范围宽,结果满意。     

Determination of olsalazine sodium in pharmaceuticals by differential pulse voltammetry

The electrochemical oxidation of olsalazine sodium was investigated by cyclic, linear sweep, differential pulse and square wave voltammetry using glassy carbon disc electrode in different buffer systems. Best results were obtained for the determination of olsalazine using the differential pulse voltammetric technique in phosphate buffer at pH 7.0. The electroactive species exhibits a diffusion-controlled voltammetric wave and its differential pulse peak current shows a linear dependence on olsalazine concentration in the range between 2 x 10(-6) M and 2 x 10(-4) M. This relationship has been applied to the determination of olsalazine in commercial capsule dosage forms. The recovery study shows good accuracy and precision for the assay developed. A UV spectrophotometric assay is also reported for comparison.     

Determination of the antibacterial trovafloxacin by differential-pulse adsorptive stripping voltammetry

A differential-pulse adsorptive stripping voltammetric method for the determination of trace amounts of the antibacterial trovafloxacin (TRFLX) is proposed. The optimal experimental parameters for the drug assay were: accumulation potential=-0.30 V (vs. Ag/AgCl), accumulation time=120 s, pulse amplitude=50 mV and scan rate=5 mV s(-1) in Britton-Robinson buffer (pH 4.5). The linear concentration range of application was 2.0-20.0 ng ml(-1) of TRFLX, with a relative standard deviation of 3.6% (for a level of 5.0 ng ml(-1)) and a detection limit of 0.6 ng ml(-1). The method was applied to determination of TRFLX in human urine and serum samples. It was validated using HPLC as a reference method. Recovery levels of the method reached 100% in all cases     

Determination of pantoprazole by adsorptive stripping voltammetry at carbon paste electrode

A voltammetric method was described for the determination of pantoprazole by differential-pulse adsorptive stripping voltammetry at a carbon paste electrode. Accumulation of pantoprazole was found to be optimized in Britton-Robinson buffer (0.04 M, pH 4.0) solution following 5 min accumulation time at open circuit condition. Under optimized conditions, the current showed a linear dependence with concentration in the range 1.0 x 10(-7)-1.0 x 10(-5) M. The detection limit was 2.0 x 10(-8) M. The method was applied successfully for the analysis of pantoprazole in tablet dosage form. The results of accuracy and precision were comparable to those obtained by spectrophotometry.     

Determination of cefonicid in human urine by adsorptive square-wave stripping voltammetry

The adsorption behavior of cefonicid on the hanging mercury drop electrode (HMDE) has been examined using cyclic voltammetry and square-wave voltammetry techniques in Britton-Robinson (B-R) buffers in the pH range of 2.0-11.0. The effect of different parameters on the accumulation behavior of the adsorbed species has been evaluated. Sensitive measurements can be achieved after controlled adsorption on the surface of HMDE followed by square-wave voltammetry. Under optimal conditions, a detection limit of 4.0 x 10(-8) M and a linear calibration graph in the range 1.0 x 10(-7)-1.0 x 10(-6) M were obtained. Direct simple determination of cefonicid in urine was established with no manipulation of urine sample other than dilution and subsequent adsorptive stripping voltammetric determination. The detection limit of the method was 1.0 microg x ml(-1) of cefonicid in urine.     

线性扫描溶出伏安法测量栽培生药中的乙硫磷农药

乙硫磷本身没有电化学活性,而在强碱性条件下它的水解产物在汞电极上具有电化学活性,在pH8·3Britton-Robinson缓冲溶液中,可获得灵敏的还原峰,峰电位为-690mV(vs.Ag/AgCl)。峰电流与乙硫磷的浓度在0·02～0·16μg/ml范围内呈线性关系,检出限为0·0087μg/ml。该文还初步探讨了乙硫磷的电化学行为。     

Determination of terbutaline enantiomers in human plasma by coupled achiral-chiral high performance liquid chromatography

Achiral-chiral column switching HPLC assay was developed to allow the separation and quantification of the enantiomers of terbutaline in human plasma by means of fluorescence detection. Plasma samples were prepared by solid-phase extraction with sep-pak silica, followed by HPLC assay. The enantiomers of terbutaline and the internal standard were separated from the biological matrix on a silica column, and the two enantiomers were resolved and quantified on a Sumichiral OA-4900 column. The two columns were connected by a switching valve equipped with silica trap column. The trap column was used to concentrate the terbutaline in the eluent from the achiral column before back flushing onto the chiral phase. For each enantiomers, the assay was linear between 2.5-125 ng/ml (r=0.9999) and detection limit was 1.0 ng/ml.     

Determination of verapamil by adsorptive stripping voltammetry in urine and pharmaceutical formulations

A sensitive reduction peak of verapamil is obtained by adsorptive stripping voltammetry in 0.01 M phosphate (pH 7.4) at an accumulation time of 30 s. The peak potential is -1.81 V (vs. Ag/AgCl). The peak current is directly proportional to the concentration of verapamil (1x10(-8)-1x10(-6) M), with a 3sigma detection limit of 5x10(-10) M (0.246 ng/ml). The R.S.D. at the 1x10(-7) M level is 1.8%. The interference of some metal ions, and some amino acids, and the application of the method to analysis of urine, and pharmaceutical formulations are described. The method is simple (no extraction), rapid (30 s accumulation time), sensitive (the detection limit of verapamil is 0.491 ng/ml), reproducible(within day R.S.D. of 1.28-1.8%), and suitable for routine analysis of verapamil, urine, and pharmaceutical formulation.     

碳糊电极阳极吸附伏安法测定雷贝拉唑

目的:考察乳癖消巴布膏皮肤用药的安全性.方法:用健康家兔分别进行完整与破损皮肤的皮肤刺激性试验;用健康豚鼠进行皮肤过敏试验;用健康大鼠进行慢性经皮毒性试验.结果与结论:乳癖消巴布膏对家兔无皮肤刺激性.对豚鼠无致敏性,对大鼠无经皮毒性.     

Determination of nifedipine in human plasma by square wave adsorptive stripping voltammetry

A simple, sensitive and selective square-wave adsorptive stripping voltammetric method has been developed and validated for the determination of nifedipine (NIF) in plasma. The assay was performed after single extraction of NIF from alkalinised plasma into organic phase. The adsorption behaviour of NIF on a hanging mercury drop electrode (HMDE) was explored by square-wave and cyclic voltammetry. The drug was accumulated at HMDE and a well-defined peak was obtained at -730 mV versus Ag/AgCl in borate buffer of pH 9.0 including 0.01 M KCl. The linear concentration range was 2.89 x 10(-9) M-3.61 x 10(-7) M (1.00-125.01 ng ml(-1)) when using 30 s accumulation time at -300 mV. Limit of detection and limit of quantification were 1.21 x 10(-9) M (0.42 ng ml(-1)) and 2.89 x 10(-9) M (1.00 ng ml(-1)) respectively. The intra-day relative standard deviation (RSD) ranged from 1.93 to 4.12% at three concentrations and the inter-day RSDs varied from 2.53 to 6.68%. The method was applied, to the plasma of pregnant women suffering from pregnancy induced hypertension, for the determination of NIF. The percentage recoveries varied from 96.26 to 99.49%. It has been shown that NIF could be determined in the presence of its main metabolite (dehydronifedipine) by the developed method.     

Determination of 5-aminosalicylic acid in pharmaceutical formulation by differential pulse voltammetry

The oxidative behaviour of 5-aminosalicylic acid (5-ASA) has been investigated by differential pulse voltammetry using a glassy carbon electrode in different buffer systems. Linear sweep voltammetry was used to study the influence of pH on the peak current and peak potential. The solution conditions and instrumental parameters were optimized to obtain a good sensitivity. The Britton-Robinson buffer of pH 1.81 was selected as a suitable analytical medium in which 5-ASA exhibited a sensitive diffusion controlled oxidative peak at 0.564 V (vs. Ag/AgCl). The peak current varied linearly with drug concentration in the range between 1 x 10(-4) and 2 x 10(-6) M. The proposed voltammetric method has been applied to the determination of the drug in commercial delayed-release tablet forms. A mean recovery of 101.23% with a relative standard deviation of 1.35% was obtained.     

"Determination of domperidone in tablet dosage form by anodic differential pulse voltammetry"

A differential pulse voltammetric method was described for the determination of domperidone. The method was based on the anodic oxidation of domperidone on a glassy carbon electrode at +0.64 V vs. SCE in Britton-Robinson buffer solution of pH 2.3. The reversibility of the oxidation was tested by cyclic voltammetry; the electrode process is irreversible and diffusion-adsorption controlled. Calibrations are linear over the range 1.0 x 10(-6)-2.0 x 10(-5) M of domperidone with a detection limit of 4.0 x 10(-7) M. The method was applied, without any interference from the excipients, to the determination of the drug in a tablet dosage form.     

Determination of amlodipine in pharmaceutical formulations by differential-pulse voltammetry with a glassy carbon electrode

A differential-pulse voltammetric method was developed for the determination of amlodipine based on the oxidation of the dihydropyridine group on the surface of glassy carbon electrode under stationary and rotating conditions. The experiments were conducted in a supporting electrolyte consisting of 0.2 M KCl, 0.1 M phosphate buffer, and 10% (v/v) methanol during investigation of initial potential and pH effects. No adsorption effect was observed on using an initial potential of 0 mV and the supporting electrolyte solution at pH 5.5 under both stationary and rotating conditions. The factor affecting the voltammetric current was diffusional in the range of 200-1000 rpm for rotating, and 2-40 mV s-1 for stationary conditions up to a concentration of 0.04 mg mL-1 amlodipine. The limit of detection (LOD) and the limit of quantitative (LOQ) for the rotating and stationary techniques were found to be 0.004 and 0.0072 mg mL-1 (for S/N = 3.3) and LOQ 0.012 and 0.022 mg mL-1 (for S/N = 10), respectively. The proposed method was applied to the tablets containing amlodipine and according to the statistical evaluations acceptable results were obtained at the 95% probability level.