Development of Validated Chromatographic Methods for the Simultaneous Determination of Metronidazole and Spiramycin in Tablets

Two chromatographic methods have been described for the simultaneous determination of metronidazole (MET) and spiramycin (SPY) in their mixtures. The first method was based on a high performance thin layer chromatographic (HPTLC) separation of the two drugs followed by densitometric measurements of their spots at 240 nm. The separation was carried out on Merck TLC aluminum sheets of silica gel 60 F₂₅₄ using methanol: chloroform (9:1, v/v) as a mobile phase. Analysis data was used for the linear regression line in the range of 1.0–2.0 and 0.8–2.0 μg band⁻¹ for MET and SPY, respectively. The second method was based on a reversed-phase liquid chromatographic separation of the cited drugs on a C-18 column (5 μm, 250 × 4.6 mm, i.d.). The mobile phase consisted of a mixture of phosphate buffer of pH 2.4 and acetonitrile (70:30, v/v). The separation was carried out at ambient temperature with a flow rate of 1.0 mL min⁻¹. Quantitation was achieved with UV detection at 232 nm based on peak area with linear calibration curves at concentration ranges 0.4–50.0 and 0.5–50.0 μg mL⁻¹ for MET and SPY, respectively. The proposed chromatographic methods were successfully applied to the determination of the investigated drugs in pharmaceutical preparations. Both methods were validated in compliance with ICH guidelines; in terms of linearity, accuracy, precision, robustness, limits of detection and quantitation and other aspects of analytical validation.

     

A Validated LC Method for Simultaneous Determination of Three Major Components in Entada phaseoloides

A high performance liquid chromatography method was developed for the simultaneous determination of three major active constituents in Entada phaseoloides, namely phaseoloidin (1), entadamide A (2), entadamide A-β-d-glucopyranoside (3), respectively. The samples were separated on an Aglient Eclipse XDB-C₁₈ column with gradient elution of acetonitrile and 0.3% phosphoric acid (v/v) at a flow rate of 1.0 mL min^?1 and detected at 280 nm. The three target compounds were completely separated within 10 min. All calibration curves showed good linearity (r > 0.9999) within test ranges. The reproducibility was evaluated by intra- and inter-day assays and RSD values were less than 1.04%. The recoveries were between 97.15 and 101.95%. The method was successfully applied to the analysis of three compounds in 22 commercial samples of E. phaseoloides. The results indicated that the developed LC assay was readily utilized as a quality control method for E. phaseoloides.     

Thin-Layer and Column-Chromatographic Methods for Simultaneous Analysis of Ambroxol Hydrochloride and Doxycycline Hyclate in a Binary Mixture

JPC – Journal of Planar Chromatography – Modern TLC - Two selective and reproducible methods have been established for simultaneous analysis of ambroxol hydrochloride (Amb) and...     

A Simple and Validated LC Method for the Simultaneous Determination of Three Compounds in Mikania laevigata Extracts

The Mikania genus is widely known as guaco and is used to treat fever, rheumatism, influenza and respiratory diseases. This article deals with the simultaneous quantification of three commercially available phenolic markers (o-coumaric acid, coumarin and syringaldehyde) in M. laevigata extracts, through LC-PDA. The validation data show that the method is specific, accurate, precise and robust, and also indicative of the stability of guaco extract. The method was linear, over a range of 1.25–20.0 μg mL⁻¹ for o-coumaric acid, 2.5–40.0 μg mL⁻¹ for coumarin, and 0.25–4.0 μg mL⁻¹ for syringaldehyde. The range of recovery was 94.3–96.4% for all the components, at a level of 100%.

     

Different Validated Methods for Determination of Cefditoren Pivoxil

JPC – Journal of Planar Chromatography – Modern TLC - Six, sensitive, precise and accurate methods have been developed for the determination of cefditoren pivoxil (CP). The first two...     

比值光谱—导数分光光度法同时测定纤维上的二组分混合染料

研究了用比值光谱－导数分光光度法同时测定两组分混合染料体系中分散大红ＢＷＦＬ和分散红玉ＺＧＦＬ的方法。回收率在９５．６％～１０７．５％。方法已用于分析纺织纤维上分散大红和分散红玉二元混染体系。     

A Simple and Validated LC Method for the Simultaneous Determination of Three Compounds in Mikania laevigata Extracts

The Mikania genus is widely known as guaco and is used to treat fever, rheumatism, influenza and respiratory diseases. This article deals with the simultaneous quantification of three commercially available phenolic markers (o-coumaric acid, coumarin and syringaldehyde) in M. laevigata extracts, through LC-PDA. The validation data show that the method is specific, accurate, precise and robust, and also indicative of the stability of guaco extract. The method was linear, over a range of 1.25–20.0 μg mL⁻¹ for o-coumaric acid, 2.5–40.0 μg mL⁻¹ for coumarin, and 0.25–4.0 μg mL⁻¹ for syringaldehyde. The range of recovery was 94.3–96.4% for all the components, at a level of 100%.     

Simultaneous Determination of Trace Ofloxacin and Enoxacin by TLC-Fluorescence Spectrodensitometry

Abstract

A new TLC-fluorescence spectrodensitometry method is described for the simultaneous determination of trace ofloxacin and enoxacin, using a optimized mobile phase of chloroformmethanolethyl acetatetetrahydrofuranaqueous ammonia (6:4.6:1.5:0.8:1.5, V/V). The influence of the silica gel plates previously treated with various concentrations of sodium edetate solution in various pH's are studied. Their R, values are 0.54 and 0.29 respectively. The excitation, wavelength is 335nm. The linear ranges are 0~75ng. The relative standard deviations are <6.9%. The mean recovery of the two antibiotics in body fluid ranged from 95.4% to 105.2%.     

A New Absorbance Ratio Derivative Spectrophotometry for the Simultaneous Determination of a Binary Mixture Containing Phenol and Resorcin

It is the most important problem of spectrophotometric analysis to determine two or more components in the same sample simultaneously without previous separation. In this respect, the absorbance derivative spectrophotometry is an analytical technique of great utility and offers greater selectivity than normal spectrophotometry. Recently, Salinas et al developed the absorbance ratio derivative spectra. The absorption spectrum of the mixture is divided by the absorption spectrum of a standard solution of one of the two or more components, and the first derivative of the ratio spectrum is obtained. The concentration of active component is then determined from a calibration graph obtained by measuring the amplitude at point corresponding to the minimum or maximum wavelength. In this way, the sensitivity of method is greatest.     

协同系数补偿—动力学两次标准加入法测定相互干扰的双组份

本提出了协同铲应补偿的动力两次标准加入法，讨论了相互干扰双组份同时测定的原理，研究了钙（Ⅵ）和钨（Ⅵ）催化的Ｈ２Ｏ２－Ｉ＾－动力学反应，确定了同时测定条件：［Ｈ２Ｏ２］＝９．×１０＾－３ｍｏｌ／Ｌ，［Ｉ＾－］＝１．０×１０ｍｏｌ／Ｌ，ＰＨ３．０，２５℃；为补偿钼和钨之间的协同催化效化效应，引入了协同催化系数的概念，有效地消除了吸江度对加和性的偏离。用本法同时测定样品中的钼和钨含量，回收率分别为９     

Simultaneous Determination of Ibuprofen and Diphenhydramine Citrate in Tablets by Validated LC

A stability-indicating LC method was developed for the simultaneous determination of ibuprofen and diphenhydramine citrate in pharmaceutical dosage forms. The chromatographic separation was achieved on an Inertsil ODS 3V, 150 × 4.6 mm, 5 μm, column. The mobile phase contained a mixture of 50 mM potassium dihydrogen phosphate buffer:acetonitrile:triethylamine:glacial acetic acid (55:45:0.2:0.2, v/v/v/v). This method allowed the determination of 2.85–9.14 mg mL^?1 of ibuprofen and 0.54–1.73 mg mL^?1 of diphenhydramine citrate, in a diluent consisting of pH 7.2, 50 mM potassium dihydrogen phosphate buffer:acetonitrile (40:60, v/v). The flow rate was 1.2 mL min^?1 and the detection wavelength was 260 nm. The limit of detection for ibuprofen and diphenhydramine citrate was 1.72 and 0.54 μg mL^?1 and the limit of quantification was 5.73 and 1.64 μg mL^?1, respectively. This method was validated for accuracy, precision and linearity. The method was also found to be stability indicating.     

多元校正-速差动力学分光光度法同时测定三组分有机磷农药

速差动力学分析结合化学计量学对动力学数据进行解析计算, 可扩大动力学分析的范围, 提高分析的准确度. 本文利用对硫磷、甲基对硫磷和杀螟硫磷在碱性介质中能与氧化剂过氧化氢发生氧化反应生成对硝基苯酚的性质, 引入多元校正方法中的经典最小二乘法(CLS)、偏最小二乘法(PLS)和主成分回归法(PCR)对动力学数据进行解析, 实现了三组分人工合成样品的同时测定.     

Validated TLC and HPLC Stability-Indicating Methods for the Quantitative Determination of Dapsone

JPC – Journal of Planar Chromatography – Modern TLC - Two stability-indicating chromatographic methods were developed for the analysis of dapsone in presence of its oxidative...     

Validated HPTLC Method for Simultaneous Determination of Loratadine and Desloratadine in Presence of Co-Formulated Drug

JPC – Journal of Planar Chromatography – Modern TLC - A highly validated and selective high performance thin layer chromatography (HPTLC) method was developed for the determination of...     

Validated HPTLC Method for Simultaneous Determination of Shanzhiside Methyl Ester and Barlerin in Barleria prionitis

JPC – Journal of Planar Chromatography – Modern TLC - Aerial parts of Barleria prionitis Linn. (Acanthaceae) have shown anti-respiratory syncytial virus, anti-arthritic,...     

鸡组织中3种青霉素类药物残留检测的前处理方法比较研究

采用高效毛细管电泳(HPCE)分离紫外检测方法,比较了乙腈萃取、乙腈萃取-固相萃取(SPE)、基质固相分散萃取(MSPD)和MSPD - SPE 4种方法对鸡组织样品中青霉素、氨苄青霉素、阿莫西林残留的前处理效果.结果表明,与其他方法相比,MSPD方法的回收率高、图谱背景干净.据此建立了鸡组织中青霉素、氨苄青霉素、阿莫...     

速差动力学分析法同时测量钆-镝混合物中的单一稀土

本文研究了稀土与新稀土显色剂DBC偶氮胂络合反应的动力学行为。稀土与试剂反应速率常数随着原子序数的增加而减小,发现了稀土动力学特性中的"钆断"现象。推导了钆、镝的动力学方程,提出了同时测量钆、镝二元混合物的速差动力学分析方法。测量了钆、镝相对浓度比为1:10-10:1的混合物试样,最低可测浓度为10^-7M,最大测量误差为13.5%。     

鼻可灵喷雾剂中地塞米松磷酸钠、氧氟沙星及盐酸麻黄碱含量的微乳液相色谱法测定

建立了复方鼻可灵喷雾剂中3 组分的微乳液相色谱(MELC)测定方法,并考察了其影响因素.以微乳(33 g/L SDS-1.2%(体积分数)正辛烷-9%(体积分数)正丁醇-0.5%(体积分数)三乙胺,磷酸调pH至3)为流动相,采用Hypersil BDS C18 5 μm(4.6 mm×150 mm)色谱柱,检测波长256 nm.实验发现,被测组分地塞米松磷酸钠、氧氟沙星及盐酸麻黄碱的线性范围和相关系数分别为0.01 ～0.04 g/L,r＝0.999 9;0.1 ～0.3 g/L,r＝0.999 9;0.2 ～0.6 g/L,r＝0.999 9.对应的平均回收率和RSD(n=5)分别为97%,2.55%;101%,0.45%;101%,0.54%(n=5).     

Validated Chromatographic Methods for the Determination of Process Related Toxic Impurities in Pantoprazole Sodium

A GC–MS method for the simultaneous determination of two process related toxic impurities viz. 2-(chloromethyl)-3,4-dimethoxypyridine hydrochloride (CDP) and dimethyl sulfate (DMS) and RP-LC for the routine determination of CDP in pantoprazole sodium (PPS) are presented. In GC–MS, a temperature gradient program was performed on a capillary DB-624 column (60 m × 0.32 mm × 1.8 μm). LC analysis of CDP was done on a Novaflex C18 (250 × 4.6 mm, 5 μm) column using mobile phase containing buffer (0.02 M potassium dihydrogen phosphate and 0.0025 M di potassium hydrogen phosphate) and acetonitrile in 46:54 v/v ratio. The flow rate was 1.0 mL min^?1 and the elution was monitored at 220 nm. Both methods were validated as per International Conference on Harmonization (ICH) guidelines. GC–MS is able to quantitate up to 3.0 ppm of CDP and DMS whereas with RP-LC up to 9.0 ppm of CDP could be quantitated.     

A Validated TLC-Densitometric Method for the Simultaneous Determination of Formoterol Fumarate and Budesonide in Pressurized Metered-Dose Inhaler

JPC – Journal of Planar Chromatography – Modern TLC - A simple and robust thin-layer chromatography (TLC) method has been developed and validated for the simultaneous quantitative...