Development and Validation of an HPLC Method for Determination of Ceftiofur Sodium

An isocratic high-performance liquid chromatographic method has been developed for assay of ceftiofur sodium in drug substance and in sterile powder for injection. Chromatography was performed on a 250 mm × 4.6 mm, 5 μm particle, C₁₈ column with a 78:22 (v/v) mixture of 0.02 m disodium hydrogen phosphate buffer (pH adjusted to 6.0 with 85% orthophosphoric acid) and acetonitrile as mobile phase, at a flow rate of 1.0 mL min⁻¹. The separation was monitored by UV detection at 292 nm. Validation of the method for linearity and range, intra- and inter-day precision, accuracy, specificity, recovery, robustness, and limits of quantification and detection yielded good results. The calibration plot was linear from 20.0–120.0 μg mL⁻¹ and the correlation coefficient was 0.9999. It was shown that ceftiofur was degraded under acidic, alkaline, oxidative, and photolytic conditions. The method was found to be stability-indicating and could be used for routine analysis of ceftiofur sodium for injection.     

导数分光光度法直接测定环境水中的十二烷基苯磺酸钠

用四阶导数分光光度法,无需经显色与萃取便可直接测定环境水中十二烷基苯磺酸钠的含量。本法抗干扰能力较强,检出限为0.7mg/l(即2×10~(-6)M),回收率为96～103%。     

Simultaneous Spectrophotometric Estimation of Rabeprazole Sodium and Itopride HCl

Abstract

Two simple, rapid, accurate, and economical analytical methods have been developed for the simultaneous estimation of Rabeprazole Sodium and Itopride Hydrochloride in combined capsule dosage form. First method is based on the determination of Q‐value and second method is based on simultaneous equation method. Rabeprazole Sodium has absorbance maxima at 284 nm and Itopride Hydrochloride has absorbance maxima at 258 nm in methanol AR. The absorption ratio (Q‐value) was determined at 266.6 nm (Iso‐bestic point) and 284 nm (λmax of Rabeprazole Sodium). Both the drugs obey Beer's law in the concentration ranges employed for these methods. Both the methods were found to be simple, rapid, accurate, and can be adopted in routine analysis of drugs in formulations. The accuracy and reproducibility of the proposed method was statistically validated by recovery studies     

Spectrophotometric Methods for the Determination of Acediasulfone in Mixture with Cinchocaine

Abstract

Derivative spectrophotometry techniques (ratio‐spectra first derivative and zero‐crossing first derivative) were described for simultaneous determination of acediasulfone and cinchocaine. Acediasulfone was also determined via the formation of a colored product as a result of its reaction with p‐dimethylaminobenzaldehyde. In the ratio‐spectra first derivative method, the measurements were taken at 310 and 233.9 nm for acediasulfone and cinchocaine, respectively. By the zero‐crossing first derivative method, lines of regression were taken at 318 and 233 nm for acediasulfone and cinchocaine, respectively. In the colorimetric method, absorbance measurements were obtained at 452 nm. Acediasulfone showed linearity over concentration ranges 2–14 µg/ml, 2–16 µg/ml, and 12–60 µg/ml for ratio‐spectra first derivative, zero‐crossing first derivative, and colorimetric methods, whereas cinchocaine showed linearity over concentration ranges 1–10 µg/ml and 2.28–16 µg/ml for ratio‐spectra first derivative and zero‐crossing first derivative techniques. The proposed methods proved to be specific and accurate for the analysis of the cited drugs in laboratory‐prepared mixtures and dosage form. The obtained results agree statistically with those obtained by reference methods.     

First Derivative Spectrophotometric Determination of Certain Drugs in Two-Component Mixtures

Abstract

Four two-component mixtures have been assayed using both Vierordt's and first derivative spectrophotometric methods. Such mixtures are acepifylline and phenobarbitone, phenylbutazone and amidopyrine, procaine and caffeine, and sulphamethoxazole and trimethoprim. These selected applications illustrate the relative ease and simplicity offered by first derivative spectrophotometry for the assay of two component mixtures with spectral interferences from matrix formulations.     

Determination of Candesartan Cilexetil in Tablet Dosage Forms and Dissolution Testing Samples by First Derivative UV Spectrophotometric Method

Abstract

This article describes the development and validation of a first derivative UV quantitative analytical method for determination of candesartan cilexetil in tablet dosage forms. A signal at 270.1 nm of the first derivative spectrum (ID_270.1) was found adequate for quantification. The limit of quantification was 3.06 µg/ml. The linearity between ID_270.1 nm and concentration of candesartan cilexetil in the range of 6.00–32.00 µg/ml presented a correlation coefficient of (r²) = 0.9990. The mean recovery percentage was 100.97 and 99.23% for candesartan cilexetil standard solution and candesartan standard cilexetil solution with excipients, respectively. The intraday and interday accuracy of the assay was 98.60% and 99.10% respectively. The intraday and interday variability was below 2.0%.

The proposed method is accurate, precise, sensitive, and selective and can be used in quality control laboratories for its intended purpose.     

Validation of UV Spectrophotometric Method for Fexofenadine Hydrochloride in Pharmaceutical Formulations and Comparison with HPLC

Abstract

A simple, reproducible, accurate, and effective spectrophotometric method was developed and validated for the quantitation of the antihistamine fexofenadine in capsules and coated tablets. Ethanol was used as solvent and the absorbance at the wavelength of 220 nm was employed to the quantitation of the drug. The method validation was fulfilled through the evaluation of the analytical parameters of linearity, precision, accuracy, limits of detection, and quantitation and specificity. The method was linear (r=0.9999) at concentrations ranging from 8.0 to 20.0 µg ml^?1, precise (RSD intra‐day=0.29; 0.18; 0.39; RSD inter‐day=0.12 for capsules and RSD intra‐day=0.13; 0.16; 0.13; RSD inter‐day=0.13 for coated tablets), accurate (percentage recovery=99.97% for capsules and 100.51% for tablets), sensitive (limits of detection and quantitation of 0.10 and 0.29 µg ml^?1, respectively) and specific. The method was compared to a high performance liquid chromatography (HPLC) method, which was previously developed to the same drug. The results showed no significant difference between the methods in fexofenadine hydrochloride quantitation.     

Spectrophotometric Determination of Phenytoin Sodium in Pure and Pharmaceutical Preparations

 Phenytoin sodium reacts with o-nitrobenzoic acid in alkaline media after heating for 10 minutes at 70 °C, to give a red coloured complex having maximum absorbance at 510 nm. The reaction is selective for phenytoin sodium with 0.01 mg/10 mL as visual limit of quantitation and provides a basis for a new spectrophotometric determination. The colour reaction obeys Beer’s law from 0.01 mg to 3 mg/10 mL of phenytoin sodium and the relative standard deviation is 0.29%. The quantitative assessment of tolerable amounts of other drugs is also studied. Received May 2, 2000. Revision May 11, 2001.     

Validation of an HPLC Analytical Method for Determination of Pancuronium Bromide in Pharmaceutical Injections

Abstract

Pancuronium bromide is used with general anesthesia in surgery for muscle relaxation and as an aid to intubation. A high performance liquid chromatographic method was fully validated for the quantitative determination of pancuronium bromide in pharmaceutical injectable solutions. The analytical method was performed on an amino column (Luna® 150 mm × 4.6 mm, 5 µm). The mobile phase was composed of acetonitrile:water containing 50 mmol L^?1 of 1-octane sulfonic acid sodium salt (20:80 v/v) with a flow rate of 1.0 mL min^?1 and ultraviolet (UV) detection at 210 nm. The proposed analytical method was compared with that described in the British Pharmacopoeia.     

Determination of Some Cephalosporins Using Derivative Spectrophotometry

Abstract

A rapid and simple method for the determination of cephalexin, cephalothin sodium and cephradin without prior separation from their alkali-induced degradation products is presented. By measuring the values of the first and second derivative spectra at certain wavelengths, the concentration of the intact drug can be calculated directly without interference of degradation products. The method was proved using synthetic mixtures of the intact drugs with their degradation products, and its suitability to monitor the stability of the drugs was demonstrated.     

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。     

亚甲基蓝分光光度法测定锑浸出液中硫化钠

湿法炼锑中常采用硫化钠作为从锑矿中提取锑硫化物的浸出剂。准确测定锑浸出液中的硫化钠浓度对掌握和完善湿法炼锑工艺、提高生产效率有重要作用。将亚甲基蓝分光光度法用于锑浸出液中硫化钠的测定,考察了波长选择、体系酸度、显色时间、基质干扰等条件,测评、优化了方法;将方法应用于锑浸出液中硫化钠的测定,方法检出限为0.002mg/L,测定结果相对标准偏差≤3%,加标回收率≥90%。方法能较理想地应用于锑浸出液中硫化钠的测定,丰富了锑浸出液中硫化钠的测定方法,也为相关研究提供了支持与参考。     

比光谱导数分光光度法同时测定微量磷和砷

采用比光谱导数法对严重重叠的砷钼酸和磷钼酸与乙基罗丹明Ｂ的缔合物的吸收光谱进行数据解释。结果表明，此法不需分离和掩蔽而能实现对微量砷和磷的同时测定，探讨了显色条件，测定波长及求导计算时波长间距的选择等问题，应用于合成样品和水样的分析。     

亚甲基蓝分光光度法测定锑浸出液中硫化钠

湿法炼锑中常采用硫化钠作为从锑矿中提取锑硫化物的浸出剂。准确测定锑浸出液中的硫化钠浓度对掌握和完善湿法炼锑工艺、提高生产效率有重要作用。将亚甲基蓝分光光度法用于锑浸出液中硫化钠的测定,考察了波长选择、体系酸度、显色时间、基质干扰等条件,测评、优化了方法;将方法应用于锑浸出液中硫化钠的测定,方法检出限为0.002mg/L,测定结果相对标准偏差≤3%,加标回收率≥90%。方法能较理想地应用于锑浸出液中硫化钠的测定,丰富了锑浸出液中硫化钠的测定方法,也为相关研究提供了支持与参考。     

十二烷基苯磺酸钠与苯酚的导数同步荧光法同时测定

研究了十二烷基苯磺酸钠和苯酚及其混合物在pH 6.0的磷酸二氢钠-磷酸氢二钠缓冲液中的一阶导数同步荧光光谱,确定了最佳实验条件:波长差Δλ=60 nm,十二烷基苯磺酸钠的测定波长为224 nm,苯酚的测定波长为258 nm,建立了一阶导数同步荧光法同时测定混合物中十二烷基苯磺酸钠和苯酚的新方法。十二烷基苯磺酸钠和苯酚的线性范围分别为0.05~8.00 mg/L和0.10~5.50 mg/L;线性相关系数分别为0.995 5和0.999 7;检出限分别为8.4μg/L和5.3μg/L;回收率分别为95%~100%和98%~102%;相对标准偏差分别为3.8%和1.9%。该方法可用于水中十二烷基苯磺酸钠和苯酚的同时检测,结果满意。     

多波长线性回归导数分光光度法同时测定饮料中糖精钠和苯甲酸

测定了同时测定两组分的多波多线性回归导数分光光度法,无需进行化学分离。方法用于模拟样品和饮料样品中糖精钠和苯甲酸的同时测定,回收率为９８％￣１０１％,相对标准偏差〈３．０％。     

Development and Validation of Spectrophotometric Methods for the Determination of Cefetamet in Pharmaceutical Dosage Forms

Two simple and sensitive spectrophotometric methods for the determination of cefetamet in either pure form or in its pharmaceutical formulations were described. The method Ⅰ is based on the interaction of 3-methylbenzo[d]- thiazolin-2-one hydrazone （MBTH） with cefetamet in the presence of freshly prepared ferric chloride in a neutral medium. The resulting blue colored product has λmax at 628 nm. The method Ⅱ describes the reduction of ferric ion by the drug to ferrous ion followed by a complex formation reaction with 1,10-phenanthroline （1,10-phen） to form an orange red colored chromogen exhibiting 2max at 510 nm. The products are stable for more than 5 and 8 h respectively. Common excipients used as additives in pharmaceutical preparations do not interfere in the proposed methods. Both methods are highly reproducible and have been applied to a wide variety of pharmaceutical preparations and the results are comparable with those of official methods.     

Development and Validation of Selective Spectrophotometric Methods for the Determination of Pregabalin in Pharmaceutical Preparation

Three simple, quick and sensitive methods are described for the spectrophotometric determination of pregabalin (Pgb) in pharmaceutical preparations. Among them, the first two methods are based on the reaction of Pgb as n-electron donors with 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ) and 7,7,8,8-tetracyanoquinodimethane (TCNQ) as π-acceptors to give highly colored complex species. The colored products were quantitated spectrophotometrically at 494 and 841 nm for DDQ and TCNQ, respectively. Optimization of the different experimental conditions was conducted. Beer’s law was obeyed in the concentration ranges 2.0—30.0 and 1.5—10 µg•mL－1 for DDQ and TCNQ methods, respectively. The third method is based on the interaction of ninhydrin (NN) with primary amine present in the pregabaline. This reaction produces a blue coloured product in N,N-dimethylformamide (DMF) medium, which absorbs maximally at 573 nm. Beer’s law was found in the concentration range 40.0—180.0 μg•mL－1. The methods were applied successfully to the determination of this drug in pharmaceutical dosage forms.     

二阶导数紫外分光光度法测定混合物中烷基酚聚氧乙烯醚和烷基苯磺酸钠

用二阶导数紫外分光光度法直接测定混合物中烷基酚聚氧乙烯醚和烷基苯磺酸钠的含量。此法不需经任何分离手续,快速、简便、准确,标准偏差±0.01,回收率在98%以上。