Current Status of Polyamine and Polyamine Analogs Analysis in Cancer Research

The amino-acid-derived polyamines have been associated with cell growth and cancer and their concentrations in malignant tumors are extremely high compared to those in tissues that are histologically normal. Hence, polyamines have been considered as an interesting object for anticancer therapy. Analysis of polyamine levels in biological fluid can possibly provide helpful information on the types of cancer and progression phase of the disease. Numerous modern analytical methods, including high-performance liquid chromatography, gas chromatography, capillary electrophoresis, and other separation techniques have been widely utilized for analysing polyamine levels. In both tissue culture and experimental animal models, polyamine analogues restrain cell growth and destroy malignant cells. Determination of intracellular analogue contents is also crucial, since analogue accumulation is a causal factor for their antitumour effectiveness. In this review, the latest methods reported for polyamines and polyamine analogs in cancer research are discussed

DEVELOPMENT AND VALIDATION OF A STABILITY-INDICATING ULTRA-FAST LIQUID CHROMATOGRAPHIC ANALYSIS FOR THE SIMULTANEOUS DETERMINATION OF FENTICONAZOLE AND ITS RELATED SUBSTANCES IN PHARMACEUTICAL FORMULATIONS

A precise stability-indicating an ultra-fast liquid chromatographic method was developed for determination of fenticonazole and its related substances in pharmaceutical formulations. Chromatographic separation was achieved on a C18 column (100 x 4mm, 3 mu m) under gradient elution by using mixture of 85% phosphoric acid solution adjusted to pH 3.0 using triethyamine and acetonitrile at a flow rate of 0.8 mL per minute. The analytes were detected using photodiode array detector at 235 nm. The retention time for fenticonazole was about 7.5 min. The drug was subjected to different stress conditions like hydrolysis (acid, alkaline and neutral), oxidation, photolysis and thermal degradation in accordance to ICH guidelines. A minor degradation was observed during oxidative hydrolysis. No degradation was observed under the other stress conditions. The method was validated for specificity, linearity, precision, accuracy, robustness, and system suitability. The method was linear in the drug concentration range of 5-150 mu g/mL with the correlation coefficient being 0.9985. The relative standard deviation for precision was below 2%. The mean recoveries were between 99.12-100.47% for drug substance. According to the obtained results, the method can successfully be applied for routine quality control analysis of fenticonazole in pharmaceutical formulation

Determination of Eprosartan Mesylate and Hydrochlorothiazide in Tablets by Derivative Spectrophotometric and High-Performance Liquid Chromatographic Methods

Two new simple and selective assay methods have been presented for the analysis of eprosartan mesylate (EPR) and hydrochlorothiazide (HCT) in pharmaceutical formulations. The first method is based on first-derivative ultraviolet spectrophotometry with zero-crossing measurements at 246 and 279 nm for EPR and HCT, respectively. The assay was linear over the concentration ranges 3.0-14.0 mu g/mL for EPR and 1.0-12.0 mu g/mL for HCT. The quantification limits for EPR and HCT were found to be 1.148 and 0.581 mu g/mL, respectively, while the detection limits were 0.344 pg/mL for EPR and 0.175 mu g/mL for HCT. The second method involved isocratic reversed-phase liquid chromatography using a mobile phase composed of acetonitrile-10 mM phosphoric acid (pH 2.5) (40:60, v/v). Olmesartan was used as internal standard and the substances were detected at 272 nm. The linearity ranges were found to be 0.5-30 and 0.3-15.0 mu g/mL for EPR and HCT, respectively. The limits of detection were found to be 0.121 mu g/mL for EPR and 0.045 mu g/mL for HCT. The limits of quantification were found to be 0.405 and 0.148 mu g/mL for EPR and HCT, respectively. The proposed methods were successfully applied to the determination of commercially available tablets with a high percentage of recovery and good accuracy and precision

Two Simple and Rapid Spectrophotometric Methods for the Determination of a New Antihypertensive Drug Olmesartan in Tablets

Two simple, rapid and reproducible spectrophotometric methods have been described for the assay of olmesartan (OLM) in pharmaceutical formulation. The methods are based on the formation of ion associates in the reactions between the studied drug substance and ion-pair agents [bromocresol green (BCG) and bromophenol blue (BPB)]. By the extraction with dichloromethane and chloroform, yellow-colored ion associates were formed in acidic medium and absorbances were measured at 409 (BCG) and 412 nm (BPB). Optimizations of the reaction conditions were performed. Beer's law was obeyed within the concentration range from 1-40 mu g/mL and 10-120 mu g/mL,respectively, for BCG and BPB. The molar absorptivity, detection and quantification limits were also determined. The developed methods were applied successfully to the determination of this drug in tablets

Spectrophotometric Determination of Antidepressant Drug Duloxetine in Pharmaceutical Preparations using pi-Acceptors

In this study, two simple and accurate spectrophotometric methods were presented for the determination of duloxetine hydrochloride (DLX) in pharmaceutical preparations. The methods were based on the reaction of DLX as n-electron donor with 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ) and 7,7,8,8-tetracyanoquinodimethane (TCNQ) as pi-acceptors to give highly colored complex species. The colored products were quantitated spectrophotometrically at 477 and 841 for DDQ, TCNQ, respectively. All variables were studied in order to optimize the reaction conditions. Beer's law was obeyed in the concentration ranges 10.0-50.0 and 15-60 mu g mL(-1) for DDQ and TCNQ method, respectively. The proposed methods have been successfully applied to the pharmaceutical analysis without any interference from excipients. The suggested procedures could be used for the determination of DLX in pharmaceutical preparations being sensitive, simple and selective

A Review of Current Methods for the Determination of Acrylamide in Food Products

Acrylamide (AA) is a potentially carcinogenic substance which is formed during heating of food products containing carbohydrates and asparagine. It was first detected in food products in 2002. Since that time, several analytical methods have been made available for the quantification of AA in various foods. Starting from the announcement in 2002, occurrence, formation, chemistry, toxicology, and potential health risk in the human diet have been investigated and methods of analysis have been reviewed in many articles. In this paper, current information and analytical methods for the determination of AA have been reviewed

High-performance Liquid Chromatography Analysis of Nebivolol and Amlodipine and Some Related Compounds in Synthetic Mixture

Objective: This study aimed to develop and validate a method using a high-performance liquid chromatography (HPLC) to perform a quantitative analysis of nebivolol (NEB) and amlodipine (AML) along with some related substances in the synthetic mixture

Ultra fast liquid chromatographic analysis of nonsteroidal anti-inflammatory drugs with fluorimetric detection in tap water, urine, and pharmaceutical samples

A novel analytical method based on ultra-fast liquid chromatography using fluorimetric detector was developed and validated for determination of non-steroidal anti-inflammatory drugs (NSAIDs) (ibuprofen (IBP), etodolac (ETD), dexketoprofen (DKP), sodium diclofenac (SDCF), and naproxen (NPX) in tap water, urine and pharmaceutical samples. Precolumn derivatisation of targeted NSAIDs was carried out with 4-bromomethyl-7-methoxy coumarin (BrMmC) using dibenzo-18-crown-6-ether as reaction catalyst leading to the formation of a fluorescent compound. The obtained fluorescent compound of NSAIDs were measured at excitation wavelength as 325 nm, and emission wavelength of 395 nm. Optimum analytical conditions were carefully studied and improved. C18 column, with the dimensions of 4.0 x 100 mm and 3 mu m particle size, was used. Gradient elution with methanol: water 40:60; v/v (eluent A) and acetonitrile 100% (eluent B) were used as mobile phase and flow rate of 0.4 mL/min. The linearity range of the analytes were between 0.01-10.0 mu g mL(-1). Recovery values obtained from pharmaceutical preparations were found as 100.04%, 99.99%, 100.09%, 99.98% and 100.47% for IBP, ETO, DKP, SDCF, NPX, respectively. LOD values were found to vary between 0.00009 mu g mL(-1) and 0.00048 mu g mL(-1) in tap water, urine and pharmaceutical samples. The optimised technique was successfully applied for the determination of NSAIDs in tap water, urine, and pharmaceutical specimen. The specified NSAIDs were not found in real tap water samples

Determination of Ciprofloxacin in Human Serum by Online Heart-Cutting Liquid Chromatography

In this study, a very simple, selective and sensitive new online heart-cutting liquid chromatographic method was developed for the determination of ciprofloxacin in human serum. The proposed method allows the determination of ciprofloxacin in human serum without complex sample preparation. The samples were mixed with methanol and filtered before analysis. Separations were performed with the following systems: the first dimension consisted of a biphenyl (50 mm x 2.1 mm) pre-separation column and the mobile phase of 25 % methanol: 75 % 30 mM ortho-phosphoric acid solution mixture, and the second dimension consisted of a C18 (150 mm x 4.6 mm) separating column and the mobile phase of 15 % acetonitrile: 85 % 50 mM ortho-phosphoric acid (pH 3.5, 100 mM triethylamine) solution mixture. The two systems were connected with a six-port valve including a 200-mu L sample loop and separations were performed continuously through injections. Detection wavelength was selected as 279 nm for both systems. The calibration curve was linear over a concentration range of 0.05-5 mu g mL(-1). The accuracy and precision of the method were determined to be 1.32-4.00 and 1.70-4.27 % ranges for RSD and RME, respectively. The absolute recovery of the drug was found to be 94.97 %. The developed method was successfully applied for the determination of ciprofloxacin in serum samples collected from a volunteer who had received 500 mg ciprofloxacin orally

LC assay of eletriptan in tablets and in vitro dissolution studies

Eletriptan (ELT) is a new selective serotonin agonist approved for the treatment of acute migraine headaches. A simple and rapid liquid chromatographic method was developed and validated for the assay of ELT in tablets. Chromatography was carried out on a 250 mm x 4.6 mm C(18) column at 30 C. Acetonitrile-15 mM triethylamine solution (adjusted to pH 7.0 using concentrated o-phosphoric acid) (60:40, v/v) mixture was used as mobile phase at 1.0 mL min(-1) flow rate and UV detector was set at 225 nm. A linear response (r(2) = 0.9999) was observed in the range of 0.1-1.6 mu g mL(-1). The method showed good recoveries (100.08 %) and the RSD values for intra- and inter-day precision were 0.78-1.93 and 1.10-2.15%, respectively. The method can be used for quality control assays and in vitro dissolution studies of ELT in tablets