Extractive Spectrophotometric Method Research Articles

Markers of Endogenous Intoxication in Rats with Diabetes Mellitus Combined with Carrageenan-Induced Enterocolitis

AbstractBackground and aims: Diabetes mellitus (DM) is a significant public health issue, being one of the major contributors to morbidity and mortality in the modern societies. Chronic hyperglycemia produces significant physiological, biochemical, and histological changes in the affected organisms. This study aims to evaluate the markers of endogenous intoxication in rats with diabetes mellitus combined with carrageenan-induced enterocolitis. Materials and methods: Diabetes mellitus was induced by a single intraperitoneal administration of streptozotocin (Sigma Aldrich, USA, at a dose of 60 mg/kg body weight). Carrageenan-induced enterocolitis was modeled by giving the animals free access to 1.0 % solution of carrageenan in drinking water for 1 month. The syndrome of endogenous intoxication was assessed by quantification of low and medium molecular weight substances in blood plasma, red blood cell suspension and urine using extraction-spectrophotometric method. Results: The increase in endogenous intoxication in streptozotocin-induced diabetes combined with chronic enterocolitis can mainly be attributed to the catabolic pool of blood plasma substances of low and medium molecular weight. The index of distribution of low- and medium-molecular-weight substances between blood plasma proteins and glycocalyx of erythrocytes in the experimental groups increased simultaneously with the quantities of investigated fractions in the erythrocyte suspension measured at the wavelengths of 242, 254 and 280 nm. Conclusions: We observed upsurge of endogenous intoxication markers in the rats with diabetes mellitus. Endotoxicosis became even more evident in the rats with diabetes mellitus combined with carrageenan-induced enterocolitis.

Determination of Fluoroquinolones in Pharmaceutical Formulations by Extractive Spectrophotometric Methods Using Ion-Pair Complex Formation with Bromothymol Blue.

In this paper, we reported a new, simple, accurate, and precise extractive spectrophotometric method for the determination of fluoroquinolones (FQs) including ciprofloxacin (CFX), levofloxacin (LFX), and ofloxacin (OFX) in pharmaceutical formulations. The proposed method is based on the ion-pair formation complexes between FQs and an anionic dye, bromothymol blue (BTB), in acidic medium. The yellow-colored complexes which were extracted into chloroform were measured at the wavelengths of 420, 415, and 418 nm for CFX, LFX, and OFX, respectively. Some effective conditions such as pH, dye concentration, shaking time, and organic solvents were also systematically studied. Very good limit of detection (LOD) of 0.084 µg/mL, 0.101 µg/mL, and 0.105 µg/mL were found for CFX, LFX, and OFX, respectively. The stoichiometry of the complexes formed between FQs and BTB determined by Job's method of continuous variation was 1 : 1. No interference was observed from common excipients occurred in pharmaceutical formulations. The proposed method has been successfully applied to determine the FQs in some pharmaceutical products. A good agreement between extractive spectrophotometric method with high-performance liquid chromatography mass spectrometry (HPLC-MS) for the determination of FQs in some real samples demonstrates that the proposed method is suitable to quantify FQs in pharmaceutical formulations.

Assay of Orphenadrine Citrate in Pharmaceuticals via Extraction-Spectrophotometric Method

An extraction-spectrophotometric technique has been applied and approved for the estimation of orphenadrine citrate in the presence of paracetamol in a binary synthetic mixture and in combined drugs. The procedure is built on the formation of a soluble red colour orphenadrine citrate – eriochrom black T (EBT) ion pair complex at pH 1.40, while the paractamol not paired. The produced red colour ion-pair complex was extracted with chloroform and showed maximum absorption at 509 nm. For quantitative evaluation Beer’s law applied to plot the absorbance against concentration, the relation was a linear in the concentration range of 0.10-6.00 µg/ mL with the molar absorptivity 4.4025 x104 L / mol. cm. The limit of detection and limit quantification were 0.024 µg/ mL, and 0.100 µg/ mL respectively. The intra-assay precision evaluated in terms of % relative standard deviation (RSD) (< 2%). And accuracy was validated with % recovery (98.8-102.5%). The results showed that orphenadrine citrate could be determined successfully in the combined tablet without interference by paracetamol and other common co-formulated substance.

THE PECULIARITIES OF THE COMPLEXATION OF Co(II) WITH 4-SULFO-2 (4'-SULFONAFTALIN-1'-AZO)-NAPHTHOL-1 IN SOLUTIONS

In this paper, the features of the complexation of the “Cobalt(II) -carmoazine-H2O2” system were studied spectrophotometrically. It is shown that the complexation of carmoazine (CAN) with Co(II) is possible only after its oxidation in the presence of hydrogen peroxide. In contrast to the previously investigated ions of variable valency metals that interact with carmoazine according to the mechanism of mutual oxidationreduction, in this case, carmoazine acts as a typical organic ligand. The optimal conditions of interaction in the investigated chemical system (pH 8, 10 vol% H2O2) were established. The complex composition (Co(III):KAN = 1:3) was determined by classical spectrophotometric methods (molar ratios and equilibrium shift). Using the Komar method molar absorbtivity of the complex was calculated (e600 = 5300). The complex stability constant which is 2.4 ∙ 109, was calculated. The presence of Co(III) ions in the newly formed as a result of the oxidation-reduction reaction to the chemical system was proved by using the intake of “interception” of trivalent cobalt ions by the competing ligand – EDTA. The charge (-6) of the product of interaction in the system “Cobalt(II) -carmoazine-H2O2” was determined by the extraction spectrophotometric method. Given the stoichiometry of the complex and the presence in the molecule of carmoazine of two negatively charged outer-sphere sulfo groups, as well as the positive charge of cation of cetylpyridinium (CP+Сl-), the composition of the ion pair extracted with chloroform [Co(III) · 3CAN2- · 6CP+] was determined. An assumption was made about the mechanism of interaction of Co (II) with carmoazine, which is preceded by the oxidation stage of Co(II) in Co(III) to form the transition peroxide complex and its subsequent complexation with carmoazine by the acid-base mechanism.

2-Nitrobenzaldehyde Thiocarbohydrazone Assisted Precise Extraction Spectrophotometric Method for the Determination of Ruthenium(III) in Alloy and Catalysts

A simple, rapid, selective, sensitive and reliable extractive spectrophotometric method was developed for the determination of ruthenium(III) using 2-nitrobenzaldehyde thiocarbohydrazone (2-NBATCH) as a chromogenic chelating ligand. The ruthenium(III)‒2-NBATCH complex is formed in aqueous acetic acid media (0.7 M) containing an organic solvent after 5 min heating on a water bath. The red colored complex is extracted into 1,2-dichloroethane and absorbance is measured at 445 nm against reagent blank. The Beer’s law is obeyed within 1‒6 g/mL of ruthenium(III), the optimum concentration range was 2‒5 g/mL of ruthenium(III) evaluated by Ringbom’s plot. Molar absorptivity and Sandell’s sensitivity of complex were 1.41 × 104 L/mol/cm and 0.0075 μg/cm2, respectively. The stoichiometry of complex was 1: 3 established from Job’s method of continuous variation, molar ratio method and logarithmic slope method. The proposed method was applied for determination of ruthenium(III) in binary and ternary, synthetic mixtures corresponding to fission product elements alloy and ruthenium(III) catalysts.

Development of an Extractive Spectrophotometric Method for Determination of Cr (VI) using 2, 4-dimethyl -3H- 1, 5 benzodiazepine

Development of an Extractive Spectrophotometric Method for Determination of Cr (VI) using 2, 4-dimethyl -3H- 1, 5 benzodiazepine

Development and Validation of an Extractive Spectrophotometric Method for Miconazole Nitrate Assay in Pharmaceutical Formulations

A simple extractive spectrophotometric technique has been developed and validated for the determination of miconazole nitrate in pure and pharmaceutical formulations. The method is based on the formation of a chloroform-soluble ion-pair complex between the drug and bromocresol green (BCG) dye in an acidic medium. The complex showed absorption maxima at 422 nm, and the system obeys Beer's law in the concentration range of 1–30 µg/mL with molar absorptivity of 2.285 × 104 L/mol/cm. The composition of the complex was studied by Job's method of continuous variation, and the results revealed that the mole ratio of drug : BCG is 1 : 1. Full factorial design was used to optimize the effect of variable factors, and the method was validated based on the ICH guidelines. The method was applied for the determination of miconazole nitrate in real samples.

Development of the UV-spectrophotometric and extraction-spectrophotometric methods of the atomoxetine quantitative determination suitable for the chemical and toxicological analysis

Development of the UV-spectrophotometric and extraction-spectrophotometric methods of the atomoxetine quantitative determination suitable for the chemical and toxicological analysis

Extractive Spectrophotometric Methods for Determination of Chlorpheniramine Maleate in Pure Form, Pharmaceutical Preparations and Biological Fluids

In this study a simple, rapid and sensitive spectrophotometric method was developed for the determination of an antihistaminic drug chlorpheniramine maleate (CPM) in pure form, pharmaceutical preparations, spiked humane urine and spiked blood serum. This method was based on the formation of ion-pairs between the basic nitrogen of the CPM drug and four chromogenic reagents namely bromocresol purple (BCP), alizarine Red S (ARS), eriochrome cyanine R (ECR), and cresol red (CR). The extracted colored ion-pairs were measured spectrophotometrically at 390, 425, 503 and 408 nm for BCP, ARS, ECR and CR reagents, respectively. The different parameters that affect the color development between CPM drug and dyestuff reagents were extensively studied to determine the optimal conditions for the assay procedure. The reaction was studied as a function of the volume of reagents, nature of solvent, temperature, reaction time and stoichiometric ratio between the CPM drug and the reagents. Beer’s law was valid over the concentration ranges of 1-30, 1-10, 2-120 and 4-120 μg mL-1 of CPM drug using BCP, ARS, ECR and CR reagents, respectively. The Sandell sensitivity, molar absorptivity, limit of detection and limit of quantification were determined. Applications of the proposed procedure to the analysis of the pharmaceutical preparations, spiked humane urine and spiked blood serum gave reproducible and accurate results without any interference from excipients. The results obtained by the proposed method were in good agreement with those obtained by reported method. The method can be suggested for the routine analysis of the cited drug.

Extractive Spectrophotometric Methods for Determination of Chlorpheniramine Maleate in Pure Form, Pharmaceutical Preparations and Biological Fluids

In this study a simple, rapid and sensitive spectrophotometric method was developed for the determination of an antihistaminic drug chlorpheniramine maleate (CPM) in pure form, pharmaceutical preparations, spiked humane urine and spiked blood serum. This method was based on the formation of ion-pairs between the basic nitrogen of the CPM drug and four chromogenic reagents namely bromocresol purple (BCP), alizarine Red S (ARS), eriochrome cyanine R (ECR), and cresol red (CR). The extracted colored ion-pairs were measured spectrophotometrically at 390, 425, 503 and 408 nm for BCP, ARS, ECR and CR reagents, respectively. The different parameters that affect the color development between CPM drug and dyestuff reagents were extensively studied to determine the optimal conditions for the assay procedure. The reaction was studied as a function of the volume of reagents, nature of solvent, temperature, reaction time and stoichiometric ratio between the CPM drug and the reagents. Beer’s law was valid over the concentration ranges of 1-30, 1-10, 2-120 and 4-120 μg mL-1 of CPM drug using BCP, ARS, ECR and CR reagents, respectively. The Sandell sensitivity, molar absorptivity, limit of detection and limit of quantification were determined. Applications of the proposed procedure to the analysis of the pharmaceutical preparations, spiked humane urine and spiked blood serum gave reproducible and accurate results without any interference from excipients. The results obtained by the proposed method were in good agreement with those obtained by reported method. The method can be suggested for the routine analysis of the cited drug.

Extractive Spectrophotometric Methods for the Determination of Dothiepin in Pure and Pharmaceutical Formulations

Extractive Spectrophotometric Methods for the Determination of Dothiepin in Pure and Pharmaceutical Formulations

Ion-pair complexes formation between fluoroquinolone antibiotics and methyl red and their use for the extraction-spectrophotometric analysis

The new spectrophotometric methods of fluoroquinolones: enrofloxacin, norfloxacin, and ofloxacin determination with the methyl red are based on ion-pair complex formation between fluoroquinolones and methyl red in acidic medium at pH 3–4 and subsequent three times extraction of the reaction products by chloroform. The obtained orange extract has an absorbance maximum at λmax = 492 nm. Optimum conditions for the formation as well as for the extraction of ion-pair complexes between fluoroquinolones and methyl red at the presence of acetate buffer and potassium chloride solutions have been established: C (CH3COONa) = 0.85 M, C (KCl) = 2 M, pH = 3.8. Effective molar absorbtivity of ion-pair complexes chloroform extracts is ɛ492∼3·103 l mol−1 cm−1. New extraction-spectrophotometric methods for fluoroquinolone determination with methyl red were developed on the basis of the optimum reaction conditions. Concentration range for the system fluoroquinolone – methyl red is (2.5–25)·10−6 M; limit of detection for enrofloxacin is Cmin = 2.48·10−6 M, for norfloxacin – Cmin = 3.07·10−6 M, for ofloxacin – Cmin = 3.17·10−6 M.

Spectrophotometric Determination of Clonazepam in Pure and Dosage forms using Charge Transfer Reaction

A rapid, sensitive and without extraction spectrophotometric method for determination of clonazepam (CLO) in pure and pharmaceutical dosage forms has been described. The proposed method was simply depended on charge transfer reaction between reduced CLO (n-donor) and metol (N-methyl-p-aminophenol sulfate) as a chromogenic reagent (π- acceptor). The reduced drug, with zinc and concentrated hydrochloric acid, produced a purple colored soluble charge-transfer complex with metol in the presence of sodium metaperiodate in neutral medium, which has been measured at λmax 532 nm. All the variables which affected the developed and the stability of the colored product such as concentration of reagent and oxidant, temperature and time of reaction were investigated and optimized. The linearity of the method was observed within a concentration range 5-40 μg ml-1 CLO and with a correlation coefficient not less than 0.998, while the molar absorbitivity and sandell sensitivity were 3.473×103 L.mole-1.cm-1 and 0.0909 μg cm-2 respectively. The present work includes also the usage of the Benesi–Hildebrand equation for the evaluation of the association constant and molar absorptivity of the colored complex .Finally the proposed method was successfully applied for the determination of CLO in tablets.&#x0D; Keywords: Spectrophotometric ; Clonazepam ; Metol ; Charge-transfer reaction.

Direct Spectrophotometric Determination of Sildenafil Citrate in Pharmaceutical Preparations Via Complex Formation with Two sulphonphthalein acid dyes

Objective: Simple, sensitive and free- extraction spectrophotometric methods have been developed for the determination of Sildenafil citrate (SIL) both in pure and in pharmaceutical forms. Methods: Two spectrophotometric methods are based on the formation of yellow colored ion-pair complexes between the studied drug and two sulphonphthalein acid dyes, bromocresol green (BCG)(method A) and bromothymol blue (BTB) (method B) with absorption maxima at 414 and 409 nm, respectively. Results: The effects of analytical parameters on the reported systems were investigated. The complexation reactions were extremely rapid at room temperature and t¬he absorption values remain unchanged up to 24h. Various analytical parameters have been evaluated and the results have been validated by statistical. Beer’s law was obeyed in the concentration ranges of (1.33 – 50) µg/ml for method A and (0.8 -27) µg/ml for method B, the limits of detection were 0.093 and 0.059 µg/ml and the molar absorptivity coefficients were 2.28×104 and 3.05 ×104 L .moL-1.cm-1 for method A and B respectively. Conclusion: The proposed methods were successfully applied to the analysis of commercial tablets containing the drugs. Two methods were free-extractive, rapid, and have high sensitivity comparing with other previous direct spectrophotometric methods. Interferences of the other ingredients and excipients were not observed.

萃取分光光度法测定钴的含量

钴与二(2-乙基己基)磷酸酯(P204)反应可生成蓝色的配合物。本文以该显色反应为基础，建立了一种新的测定钴含量的萃取光度分析法，并采用该方法测定了锂离子电池正极材料浸出液中钴的含量。对条件进行优化后，确定的最佳分析条件为：将皂化率为70%的P204溶解于环己烷中，使其浓度为30 mmol/L，加入1%(v/v)磷酸三丁酯(TBP)作相改进剂，以防止第三相的形成。待测试液用0.2 moL/L pH 5.2~5.5的HAc-NaAc缓冲溶液进行稀释。将有机相与待测试液按1:1体积比混合，转速为200 r/min的条件下萃取15 min，在627 nm处测定有机相的吸光度。钴浓度在0~250 mg/L的范围内与吸光度呈良好的线性关系，线性回归方程为A = 0.0033c-0.0377, R2 = 0.996。平均加标回收率为95.74% (加标回收率在94.36%~97.36%之间)，相对标准偏差为1.50% (n = 6)，表明该方法具有良好的准确度和精密度。干扰实验表明，共存的Ni、Mn对测定结果均无影响。 Cobalt can react with bis(2-ethylhexyl) phosphate (P204) to form blue complexes. Based on this chromogenic reaction, a new extraction spectrophotometric method for the determination of cobalt content was established. The content of cobalt in the leaching solution of cathode material of lithium ion battery was determined by this method. The operation parameters of the experiment were optimized and the optimal analysis conditions were as follows: P204 with a saponification rate of 70% was dissolved in cyclohexane at a concentration of 30 mmol/L and 1% (v/v) of tributyl phosphate (TBP) was added as a phase modifier to prevent the formation of the third phase. The test solution was diluted with 0.2 mg/L HAc-NaAc buffer solution with a pH of 5.2 to 5.5. The organic phase was mixed with the test solution at a volume ratio of 1:1; the extraction was carried out at a rotation speed of 200 rpm for 15 minutes and the absorbance of the organic phase was measured at 627 nm. The linear regression equation was A = 0.0033c-0.0377 and R2 = 0.996 in the range of 0~250 mg/L of cobalt concentration. The average recoveries were 95.74% (the recoveries ranged from 94.36% to 97.36%), and the relative standard deviation was 1.50% (n = 6), indicating that the method had good accuracy and precision. The interference experiments showed that the coexisting Ni and Mn had no effect on the determination results.

Novel Spectrophotometric Method Development for the Estimation of Boceprevir in Bulk and in Pharmaceutical Formulations

A New, Simple, Rapid and economical extractive spectrophotometric methods were developed for the determination of Boceprevir (anti-retroviral drug). Boceprevir is a direct acting protease inhibitor for the treatment of hepatitis C. It also has two isomers in which the S isomer is more active than the R-isomer. The methods were based on the formation of color chromogens with Bromo cresol green, Bromo thymol blue, Bromo phenol blue and Methyl orange indicator. The extractive spectrophotometry was carried out with phthalate buffer and chloroform. The absorbances of the chromogens were measured at 410 nm and 415 nm against the corresponding reagent blank. The proposed methods have been successfully applied to the bulk drug. The method has been statistically evaluated and was found to be precise and accurate.

NEW SPECTROPHOTOMETRY METHOD FOR THE DETERMINATION OF MIRTAZAPINE IN PHARMACEUTICAL FORMULATIONS

A simple extractive spectrophotometric method has been developed for the quantification of mirtazapine. This method is based on the formation of ion-association complex of mirtazapine drug with bromocresol purple dye. The absorbance of the complex was measured at 400 nm. The method was successfully applied to the determination of mirtazapine in their pharmaceutical formulations. The method shows a linear range from 0.2-10 μg mL -1 with a molar absorptivity of 1.53 ‘10 4 L mol -1 cm -1 . The limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.096 μg mL -1 and 0.32μg mL -1 respectively. The developed methodology was successfully applied for the determination of mirtazapine in commercial formulation and the percentage recovery was found 99.91 ± 0.15. The developed methodology promises a feasible, low cost and an efficient method for the routine analysis.

Extractive Spectrophotometric Methods for determination of Prasugrel Hydrochloride in Pharmaceutical Formulations using some Acidic Triphenylmethane Dyes

Three simple and sensitive extractive spectrophotometric methods have been described for the assay of ondansetron hydrochloride either in pure form or in pharmaceutical formulations. The developed methods involve formation of coloured chloroform extractable ion-pair complexes of the drug with bromothymol blue (BTB), bromophenol blue (BPB) and bromocresol green (BCG) in acidic medium. The extracted complexes showed absorbance maxima at 419 nm for all three methods. Beer’s law is obeyed in the concentration ranges 2.5-25, 2.5.0-25 and 3.5-22.5 µg/ml with BTB, BPB and BCG respectively. The effect of concentration of dye, pH, and interference of excipients have been studied and optimized. The limits of detection and quantification have been determined for three methods. All the three methods have been validated as per the guidelines of ICH. The methods have been applied to the determination of drug in commercial tablets and results of analysis were validated statistically through recovery studies.

Selective Spectrophotometric Determination of Trace Amounts of Cadmium in Soil and Sediment Samples Using a Green Aqueous Biphasic Extraction.

A green extraction spectrophotometric method was presented for the determination of trace amounts of cadmium in soil and sediment samples. This method is based on the selective extraction of cadmium as its iodide complex by aqueous biphasic extraction composed of polyethylene glycol (PEG) and sodium sulfate, and a subsequent sensitive determination by spectrophotometry using 2-(5-bromo-2-pyridylazo)-5-[N-n-propyl-N-(3-sulfopropyl)amino]phenol. This extraction method is simple and environmentally benign, since the organic solvents used for the traditional liquid-liquid extractions are replaced by the non-toxic polymer and inorganic salt. Cadmium can be selectively extracted from soil and sediment samples into the PEG-rich upper phase by an aqueous biphasic system containing potassium iodide and sulfuric acid. The proposed method was applied to the determination of cadmium in certified reference materials for soil and river sediment. The obtained results were in good agreement with the certified values.

Development of Extractive Spectrophotometric Method for the Determination of Osmium (IV) with Schiff base 2-[(2-Hydroxy Phenyl Imino) Methyl]-4-Nitro Phenol.

A simple spectrophotometric method has been developed for the determination of Osmium (IV) by using Schiff base 2-[(2-hydroxyphenylimino) methyl]-4-nitrophenol [HPIMNP]. HPIMNP extracts Os (IV) quantitatively (99.94%) into iso-amyl alcohol from an aqueous solution of pH range 0.0–2.0. The iso-amyl alcohol extracts show maximum absorption at 545 nm (λ max). Beer's Law is obeyed over the Os (IV) concentration range of 1.5 to 24.0 μg/ml. The Molar absorptivity and Sandell's sensitivity for Os-HPIMNP system is 3700.00L mole−1 cm −1 and 0.051μg.cm−2 respectively. The composition of extracted species is found to be 1: 3 [Os-HPIMNP] by Job's continuous variation and Mole-ratio method. Interference by various ions has been studied. The proposed method is rapid, sensitive, reproducible and accurate and it has been satisfactory applied for determination of Osmium (IV) in Synthetic mixture samples.