Determination of diazepam and otilonium bromide in pharmaceuticals by ratio-spectra derivative spectrophotometry

Binary mixtures of diazepam and otilonium bromide are analyzed by ratio-spectra first- and second-derivative spectrophotometry. The procedures are accurate, non-destructive and do not require any separation step. Calibration graphs are linear with zero-intercept up to 50 μg/ml, r ranging from 0.9996 to 0.9999. Working wavelengths in the first- and second-derivative mode, respectively, are: diazepam 247 nm and 231 nm, otilonium bromide 262 nm and 226 nm. Limits of detection (LOD) are 0.30 and 0.12 μg/ml for diazepam and 0.063 and 0.30 μg/ml for otilonium bromide. The methods were successfully applied for determining the two drugs in laboratory mixtures and in pharmaceutical products. Received: 5 August 1996 / Revised: 16 September 1996 / Accepted: 18 September 1996     

Determination of bismuth and zinc in pharmaceuticals by first derivative UV-Visible spectrophotometry

A first order derivative spectrophotometric method has been developed for the simultaneous determination of bismuth and zinc by dithizone without time-consuming extraction step. The reactions of bismuth and zinc with dithizone in a three component solution prepared in water, acetone and n-propanol mixture have been investigated. These cations react with dithizone in this mixture at pH 5.0, forming coloured complex that is stable for at least 2 h. The linear range in D evaluation was between 3.0 × 10⁻⁶ and 1.8 × 10⁻⁵ mol l⁻¹ for Zn and 2.4 × 10⁻⁶ and 1.2 × 10⁻⁵ mol l⁻¹ for Bi. The limits of detection for the analytical procedure were found 0.05 mg l⁻¹ for both cations. The relative standard deviations for the determination of 0.5 mg l⁻¹ bismuth and 0.5 mg l⁻¹ zinc were 1.2 and 1.1%, respectively, for five determinations. The procedure is simple, rapid and reliable. This method was applied to the determination of bismuth and zinc in the pharmaceutical materials successfully. Good agreement was achieved between the results obtained by the proposed and comparative methods.     

流动注射光度法测定药物中的盐酸氯丙嗪

在pH 4.04的HAc-NaAc缓冲液中, 刚果红与盐酸氯丙嗪在室温下迅速结合生成缔合物, 且缔合物在480 nm处有最大吸收. 基于此建立了流动注射光度法测定药物中盐酸氯丙嗪的含量. 方法线性范围为0.25～50.0 μg/mL, 检出限为0.082 μg/mL, 测定频率达80次/h.     

Simultaneous determination of furaltadone and chloramphenicol in pharmaceuticals by derivative spectrophotometry and the derivative of the ratio spectra

Two methods for determining furaltadone and chloramphenicol in mixtures by first derivative spectrophotometry and the derivative of the ratio spectra are described. The procedures do not require any separation step. By both methods lower determination and detection limits are obtained. The methods were applied for determining the two compounds in two pharmaceutical products.     

Determination of mixtures of ampicillin and cloxacillin in pharmaceuticals by second-derivative spectrophotometry

Mixtures of ampicillin-Na and cloxacillin-Na are assayed by peak-to-baseline and zero-crossing second-derivative spectrophotometry. The procedure does not require any separation step. Calibration plots are linear (r = 0.9999) up to 30 μg ml^?1 of ampicillin-Na at 216 nm and up to 40 μg ml^?1 ampicillin-Na or cloxacillin-Na at 228 nm or 248.8 nm, respectively, in the presence of one another. Detection limits at the p = 0.05 level of significance, range from 0.15 pg ml^?1 to 0.33 μg ml^?1. The method was successfully applied to commercial injections and capsules containing these penicillins.     

一阶导数紫外分光光度法测定羟甲基烟酰胺

研究了羟甲基烟酰胺在水、0.01mol·L-1NaOH和0.01mol·L-1HCl中的紫外吸收,通过对比,提出了以0.01mol·L-1NaOH为溶剂的一阶导数紫外分光光度法测定新方法。该法排除了赋型剂的影响,已用于片剂中羟甲基烟酰胺的测定。     

Determination of pefloxacin in serum and pharmaceutical forms by derivative spectrophotometry

A method for the direct determination of pefloxacin in serum and pharmaceutical forms (tablets and ampoules) has been developed, based on the use of second-order derivative ultraviolet spectra. Spectrophotometric assay of pefloxacin in tablets and ampoules was carried out in 0.1 mol/L NaOH, while in serum it was performed in 0.1 mol/L NaOH with the addition of sodium dodecylsulfate, in 337–347 nm wavelength range. Linear calibration curves were obtained in the concentration ranges 2–30g/mL pefloxacin for tablets and ampoules and 0.12–5 g/ mL for serum samples. Relative error of determination, as criterion for accuracy, was less than 1%, while the precision was better than 4 ng/ml. The minimum detectable concentration of pefloxacin in serum was 15 ng/mL.     

Determination of Simvastatin in tablet formulations by derivative UV spectrophotometry

An investigation of UV spectroscopic methods, i.e. absorbance, 1st and 2nd derivative spectra for the determination of simvastatin in tablet formulations has been undertaken. This work investigated the possible difficulties that might arise due to the presence of UV absorbing excipients and likely presence of degradation products in such assays. We have demonstrated that the presence of ascorbic acid as an excipient causes interference with simple absorbance measurements leading to a gross over-determination of the simvastatin. 1st and 2nd derivative methods appear to eliminate this problem. We have also shown that the degradation product of simvastatin, i.e. simvastatin β-hydroxy acid, having an almost identical spectrum to the parent drug, may cause problems in the UV spectroscopic determination of the drug in degraded samples.     

Determination of sulfamethoxazole and trimethoprim by ratio spectra derivative spectrophotometry

Summary A new method is described for analysing the binary mixture of sulfamethoxazole and trimethoprim, using the ratio spectra derivative spectrophotometry. The procedure does not require any separation step. Calibration graphs were linear up to 25 mg/l of sulfamethoxazole and up to 50 mg/l of trimethoprim; their 1:5 and 5:1 (m/m) mixtures can be resolved with recoveries between 97 and 104%. The method was satisfactorily applied for determining sulfamethoxazole and trimethoprim in different pharmaceutical products.     

Determination of astaxanthin in Haematococcus pluvialis by first-order derivative spectrophotometry

A highly selective, convenient, and precise method, first-order derivative spectrophotometry, was applied for the determination of astaxanthin in Haematococcus pluvialis. Ethyl acetate and ethanol (1:1, v/v) were found to be the best extraction solvent tested due to their high efficiency and low toxicity compared with nine other organic solvents. Astaxanthin coexisting with chlorophyll and beta-carotene was analyzed by first-order derivative spectrophotometry in order to optimize the conditions for the determination of astaxanthin. The results show that when detected at 432 nm, the interfering substances could be eliminated. The dynamic linear range was 2.0-8.0 microg/mL, with a correlation coefficient of 0.9916. The detection threshold was 0.41 microg/mL. The RSD for the determination of astaxanthin was in the range of 0.01-0.06%; the results of recovery test were 98.1-108.0%. The statistical analysis between first-order derivative spectrophotometry and HPLC by T-testing did not exceed their critical values, revealing no significant differences between these two methods. It was proved that first-order derivative spectrophotometry is a rapid and convenient method for the determination of astaxanthin in H. pluvialis that can eliminate the negative effect resulting from the coexistence of astaxanthin with chlorophyll and beta-carotene.     

Optimisation and validation of a capillary electrophoresis method for the simultaneous determination of diazepam and otilonium bromide.

A simultaneous assay of diazepam and otilonium bromide in coated tablets by capillary zone electrophoresis (CZE) was developed. The influence of various parameters (voltage, temperature, buffer concentration and pH, ethanol percentage) on analysis time and on the theoretical plates of the two peaks was investigated by means of experimental design. A response surface study was carried out by means of a 27-run D-optimal matrix. The best background electrolyte was found to be 0.13 M, pH 2.9 Britton-Robinson buffer, containing 10% v/v ethanol. Other optimised parameters were voltage (30 kV) and temperature (30 degrees C). The UV detector for quantitation of otilonium bromide and diazepam was set at 280 nm and 230 nm, respectively. Procaine hydrochloride was used as internal standard and run time was less than five minutes. Validation was performed, for drug substance and drug product, according to ICH3 guidelines. For drug product the recovery for otilonium bromide and diazepam ranged from 98.3% to 101.2% and from 97.1% to 99.0%, respectively; the RSD values found for otilonium bromide and diazepam ranged from 2.4% to 3.0% and from 1.1% to 4.5%, respectively.     

Determination of sulphamethizole in the presence of nitrofurantoine by derivative spectrophotometry and ratio spectra derivative

Two methods for determining sulphamethizol in the presence of nitrofurantoine in mixtures by first-derivative spectrophotometry and by the first derivative of the ratio spectra are described. The procedures do not require any separation step. In the first method the measurements are obtained in the zero-crossing wavelengths and the calibration graphs were linear up to 32 mug/ml of sulphamethizole at 251 and 278.5 nm. In the second method, the calibration graphs were linear up to 43 mug/ml by measuring at the maximum (263 nm), at the minimum (244 nm) and peak to peak. The methods were applied for determining sulphamethizole in a pharmaceutical product containing nitrofurantoine.     

Determination of palladium, platinum and gold by first derivative spectrophotometry

Summary The application of first-derivative spectrometry to the simultaneous determination of palladium(II), platinum(IV) and gold(III) is described. Light absorption of stable chlorocomplexes formed in 1 mol/l hydrochloric acid provides the basis of their determinations. A difference in the derivative amplitudes between two first-derivative zero crossing points of one metal A is read, corrected for the contribution of metal B and used for quantitation of metal C. Palladium (0.48–20 g ml^–1), platinum (0.16–24 g ml^–1) and gold (0.32–24 g ml^–1) have been determined with good precision and accuracy without any separations. Results are also presented for the simultaneous determination of the three precious metals in the presence of several major constituents.     

Determination of amodiaquine in pharmaceuticals by reaction with periodate and spectrophotometry or by high-performance liquid chromatography

Two methods are described for the determination of amodiaquine in pharmaceuticals. In the first method, amodiaquine was treated with periodate at pH 7.5-8.5 to yield a chromogen, which is believed to be a 1,4-benzoquinone imine derivative, and extracted into chloroform for spectrophotometric assay. The maximum molar absorptivity was found to be 2.17 x 10(3) l mol-1 cm-1 at 442 nm. Primaquine and chloroquine, if present also, do not interfere. The second method, which was used for the simultaneous determination of amodiaquine, primaquine and chloroquine, is based on high-performance liquid chromatography on an octadecylsilane column using a mobile phase of methanol-water (80 + 20) containing 0.5% anhydrous acetic acid and an over-all concentration of sodium dodecyl sulphate of 0.5 mM, with detection at 340 nm.     

Determination of attapulgite and nifuroxazide in pharmaceutical formulations by sequential digital derivative spectrophotometry

A new method for the sequential determination of attapulgite and nifuroxazide in pharmaceutical formulations by first- and second-derivative spectrophotometry, respectively, has been developed. In order to obtain the optimal conditions for nifuroxazide stability, studies of solvent, light, and temperature effects were performed. The results show that a previous hydrolysis of 2 h in 1.0 x 10(-1)M NaOH solution is necessary in order to obtain stable compounds for analytical purposes. Subsequently, the first- and second-derivative spectra were evaluated directly in the same samples. The sequential determination of the drugs can be performed using the zero-crossing method; the attapulgite determination was carried out using the first derivative at 278.0 nm and the nifuroxazide determination, using the second derivative at 282.0 nm. The determination ranges were 5.7 x 10(-6)-1.0 x 10(-4) and 3.7 x 10(-8) -1.2 x 10(-4)M for attapulgite and nifuroxazide, respectively. Repeatability (relative standard deviation) values of 1.2 and 3.0% were observed for attapulgite and nifuroxazide, respectively. The ingredients commonly found in commercial pharmaceutical formulations do not interfere. The proposed method was applied to the determination of these drugs in tablets. Further, infrared spectroscopy and cyclic voltammetry studies were carried out in order to obtain knowledge of the decomposition products of nifuroxazide.     

Determination of trace amounts of cobalt by solvent extraction--second derivative spectrophotometry

A sensitive derivative spectrophotometric method is described for the determination of microamounts of cobalt based on the integration of liquid-liquid separation and reaction, in dichloroethane, of the analyte with 3-(4-phenyl-2-pyridinyl)-5-phenyl-1,2,4-triazine (PPT) and 2,4,6-trinitro-phenol (picric acid). Cobalt was thus determined in the range 7.2-500 ng/ml. The method has a high selectivity with a detection limit of 2.2 ng/ml. The relative standard deviations were 3.2 and 1.5% for 20 and 100 ng/ml cobalt, respectively. The proposed method was applied to the determination of the analyte in vitamins.     

Determination of platinum and iridium in reforming catalysts by second derivative and absorptiometric spectrophotometry

Summary Investigations on the spectrophotometric determination of platinum as a complex formed by tin(II)chloride in hydrochloric acid are reported. The determination of platinum was found to be interfered with by iridium, because it also forms a complex with tin(II) chloride. The features of the derivative absorption spectrophotometry for the quantitative determination of platinum and iridium was also studied. The analytical application of the method for the determination of platinum and iridium in catalysts was investigated.     

Determination ofo-Cresol Red in Xylenol Orange and semi-Xylenol Orange by third-order derivative spectrophotometry

A new method is proposed for the determination ofo-Cresol Red in Xylenol Orange and semi-Xylenol Orange by third-order derivative spectrophotometry at 491 nm in a medium of 0.09 mol/1 sulphuric acid. A linear relationship exists between d³A/d³ and theo-Cresol Red concentration (1–12 g/ml), with a standard deviation of 0.11 g/ml (n = 8) for 10 g/ml ofo-Cresol Red.Presented at the 34th IUPAC Conference (1993)