High performance liquid chromatographic determination of butamyrate citrate in pharmaceutical preparation

An HPLC method was developed and validated for the determination of butamyrate citrate. The HPLC separation was achieved on a diol column (300 × 4.6 mm) packed with 5.0 μm particle size using a mobile phase of ammonium acetate buffer (pH = 6.5) and methanol (750:250, v/v) at a flow rate of 1.4 ml min^?1. The UV detector was operated at 225 nm. The method was validated for specificity, linearity, precision, accuracy and robustness. The retention time was 5.9 min. The proposed method provided linear responses within the concentration range 75–225 μg ml^?1 with LOD and LOQ values of 0.69 and 2.29 μg ml^?1, respectively. Correlation coefficient (r) of the regression equation was 0.9999. The method was found to be precise, accurate, and reproducible.     

Fluorimetric determination of mebendazole and flubendazole in pharmaceutical dosage forms after alkaline hydrolysis

The selective and very sensitive fluorimetric determination of mebendazole and flubendazole is based on alkaline hydrolysis and adsorption on Whatman 42 filter paper. Limits of detection are 0.1 μg ml^?1 and 0.5 μg ml^?1, respectively, with linear response sponse up to 10 μg ml^?1 and 50 μg ml^t?1. The fluorescence produced is very stable (λ_em = 460 nm) and the method is applicable to anthelmintic pharmaceutical preparations.     

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.     

Colorimetric Determination of Propofol in Bulk form,Dosage Form and Biological Fluids

ABSTRACT

Propofol is coupled with 2, 6-dichloroquinone-4-chlorimide (DCQ) in a reaction buffered at pH 9.6 to give a colored product having an analytically useful maximum at 635 nm. The factors affecting the color generation were optimized and incorporated in the procedure. The reacted propofol has a molar absorptivity of 3.9 × 10^?4 L mol^?1 cm^?1, and Beer's law is obeyed for concentrations 1-5 μg ml^?1 with detection limit 0.25 μg ml^?1. The method was found applicable to biological fluids (plasma and urine) spiked with propofol at concentration levels 1-5 μg ml^?1 for plasma and 1-5 μg 0.5 ml^?1 urine (less sensitivity is obtained with urine volumes above 0.5 ml) with detection limits 0.28 μg ml^?1 for plasma and 0.4 μg 0.5 ml^?1 urine. The average recovery for the commercial preparation (1% w/v propofol emulsion intravenous injection for infusion) was 99.54% with an RSD of 1.05%. The method was validated by an adopted HPLC method. The results obtained by the HPLC method for the commercial preparation were statistically compared with the proposed method and evaluated at the 95% confidence limits.     

Utility of p-chloranilic Acid and 2,3 Dichloro-5,6-dicyano p-Benzoquinone (DDQ) for the Spectrophotometric Determination of Triamterene

Abstract

Two simple and sensitive spectrophotometric procedures are suggested for analysis of triamterene. The first procedure is based on the reaction of triamterene with p-chloranilic acid (p-CA) in methylene chloride to form a highly stable coloured product, exhibiting maximum absorbance at λ 530 nm. Beer's law is obeyed in the range of 40–220 μg.ml^?1 with a mean percentage accuracy of 99.98 ± 0.446. Limit of determination is 20 μg.ml^?1. In the second procedure, the drug is determined via charge transfer complex formation with 2,3 dichloro-5,6-dicyano p-benzoquinone (DDQ) using methylene chloride as a solvent. Here the reaction product has two well defined maxima at 460 nm and 530 nm where each has been utilized for quantitative determination. Beer's law is obeyed in concentration ranges of 25–125 μg.ml^?1 and 25–150 μg.ml^?1 with mean percentage accuracies of 99.92 ± 0.449 and 100.00 ± 0.511 for both maxima. 460 and 530 nm. respectively. Limit of determination is 12.5 μg.ml^?1 at both maxima. Optimum conditions for each procedure have been studied and the stoichiometry of both reactions was ascertained using Job's method of continuous variation. The validity of the suggested procedures was assessed by applying the standard addition technique using the drug capsules. Both procedures are statistically analyzed as compared with BP method for analysis of triamterene (non aqueous titration) revealing good accuracy and precision as indicated by t and F tests.     

Selective Kinetic Spectrophotometric Determination of Nitrite in Food and Water

Abstract

A highly selective and sensitive method for the kinetic spectrophothometric determination of sub-microgram amounts of nitrite has been development based on its reaction with Nile blue 2B in acidic medium. The reaction is monitored spectrophotometrically at 595 nm at a fixed time of 4.5 min. The change in absorbance at 595 nm is related to the concentration of nitrite in the range 0.005 - 1.100 μg.ml^?1 The detection limit is 0.001 μg.ml^?1. The relation standard deviation is 1% for 0.020 μg.ml^?1 of nitrite for ten replicate measurements. Most common anions and cations do not interfere. The procedure was applied to the determination of trace amounts of nitrite in sausage and water.     

Spectrophotometric and Spectrofluorimetric Determination of Famotidine and Ranitidine Using 1,4-Benzoquinone Reagent

ABSTRACT

Spectrophotometric and spectrofluorimetric methods were adopted for the analysis of Famotidine and Ranitidine depending on their reaction with 1,4 Benzoquinone reagent at pH 5.2 and 5.6, respectively. The absorbances of the resulting condensation products were measured at 502 and 508 nm for Famotidine and Ranitidine, respectively. Concentrations adhering to Beer's law were from 40-160 μg.ml^? for Famotidine and from 20-100 μg.ml^? for Ranitidine.

Furthermore the resulting condensation products exhibited fluorescence at 665 nm when excited at 290 nm and the calibration graphs were rectilinear from 0.4-1.4 μg.ml^? for Famotidine and from 0.21 μg.ml^? for Ranitidine.

Different parameters affecting these reactions were thoroughly studied. Also these methods were applied to the pharmaceutical preparations and the results were satisfactory. The validities of the methods were ascertained by the standard addition technique revealing fine results in consideration to the mean recovery percent and standard deviation.

The spectrofluorimetric method was a hundred times more sensitive then the spectrophotometric method. The proposed methods were sensitive, accurate, and precise as statistically compared with the official methods of analysis of Famotidine and Ranitidine.     

Ion-Associates of Alkaloids and Synthetical Psychopharmaca With Cresol Red.

Abstract

Ethylmorphine, morphine, codeine, cocaine, sernyl (PCP), LSD, 3-quinuclidinyl benzilate (BZ) provide, together with Cresol Red, ion-associates that are extractable by chloroform. The extracts of the ion-associates prove the absorption maxima in the interval 405 to 415 nm. Maximum extraction of the analytes of the ion-associates is reached after 4 minutes, taking readings of different pH values in 4 intervals of 1.5. This method allows detect of alkaloids and synthetical psychopharmaca row of quantities between 0.45 μg.ml^?1 and 1.55 μg.ml^?1 and to determine 1.05 μg.ml^?1 to the amount 2.99 μg.ml^?1 of the analytes in the aqueous solutions.     

Spectrophotometric determination of L-ascorbic acid in pharmaceutical preparations

The method is based on the oxidation of L-ascorbic acid with potassium hexacyanoferrate (III). Excess of oxidant is determined spectrophotometrically by oxidation of phthalophenone to phenolphthalein in alkaline solution. Linear calibration graphs are obtained for 0–7 μg ml^?1 ascorbic acid at 553 nm, with a detection limit of 0.1 μg ml^?1. Sugars and other organic compounds do not interfere when present in moderate amounts.     

Flow Injection Analysis of Famotidine with Spectrophotometric Detection

Abstract

A flow injection determination of famotidine has been described. The method is based on the reaction of the drug with cupric acetate to form a blue coloured complex which shows absorption maxima at 314 nm and 630 nm. For an injection volume of 100 μl calibration graphs were rectilinear from 10- 50 μg. ml^?1 and 50–500 μg.ml^?1 of drug at the two wavelengths respectively. Samples could be analysed at rates upto 60 per hour with a relative standard deviation less than 1.4%. The method was evaluated by analysis of the pure drug and commercial formulations. The results compare well with those obtained by official methods.     

Determination of phosphorus in biological tissues by aluminium block digestion and flow-injection spectrophotometry

Biological tissues are digested with nitric and perchloric acids in a heated aluminium block. Flow-injection spectrophotometry is then used to measure phosphate via the phosphovanadomolybdate complex at 413 nm. The detection limit is 0.3 μg ml^?1 phosphorus; relative standard deviations are 0.7% and 0.4% at 1 μg ml^?1 and 25 μg ml^?1 phosphorus, respectively. Interferences are discussed. The decomposition procedure is evaluated for model compounds and standard reference materials.     

Fluorescent Complexes of Nucleic Acids/8-Hydroxyquinoline/Lanthanum(III) and the Fluorometry of Nucleic Acids

Abstract

The ternary fluorescent complexes of nucleic acids/8-hydroxyquinoline/ lanthanum (III) were studied. Nucleic acids in the study involve natured and thermally denatured calf thymus DNA, fish sperm DNA and yeast RNA. In the range of pH 8.0–8.4 (controlled by NH₃-NH₄Cl buffer) ternary fluorescent complexes are formed which emit at 485.0 nm for calf thymus DNA and at 480.0 nm for yeast RNA (when excited at 267.0 nm) and emits at 483.0 nm for fish sperm DNA when excited at 265.0 nm. Based on the fluorescence reactions sensitive fluorometric methods for nucleic acids were proposed. Using optimal conditions, the calibration curves were linear in the range of 0.4–3.6 μg˙ml^?1 for calf thymus DNA, 0.4–4.0 μg-ml^?1 for fish sperm DNA and 0.4–4.0 μg˙ml^?1 for yeast RNA, respectively. The limits of determination (3σ) were 0.076 μg˙ml^?1 for calf thymus DNA, 0.068 μg˙ml^?1 for fish sperm DNA and 0.329 μg˙ml^?1 for yeast RNA, respectively. Five synthetic samples were determined with satisfaction.

     

Spectrophotometric determination of iron(III) with EDTA tetrahydrazide

The tetrahydrazide of ethylenediamine tetraacetic acid (NH₂NH)₄-EDTA was synthesized from the EDTA ester and hydrazine hydrate in ethanolic solution, the resulting (NH₂NH)₄-EDTA being recrystallized in 60% ethanol. When the spectrophotometric study of the iron(III) (NH₂NH)₄-EDTA complex in aqueous solution was made two absorption maxima at 530 and 450 nm at pH 4.5 and 11.0, respectively, were found. Beer's law is obeyed in the range 1.0–20.0 μg Fe(III) ml^?1 at 530 nm and pH 4.5 and 0.5–12.0 μg Fe(III) ml^?1 at 450 nm and pH 11.0, the molar absorptivities being 1.95 × 10³ 1 mol^?1 cm^?1 at 530 nm and 3.35 × 10³ 1 mol^?1 cm^?1 at 450 nm, respectively. The Ringbom optimal interval falls between about 3 and 18 μg Fe(III) ml^?1 at 530 nm and about 2–14 μg Fe(III) ml^?1 at 450 nm. The reaction between the metal and the ligand was also investigated. The method has been successfully applied to the determination of iron in talcs.     

Spectrophotometric and First Derivative Spectrophotometric Determination of Magnesium with 1-Hydroxy-2-Carboxyanthraquinone

Abstract

1-Hydroxy-2-carboxyanthraquinone reacts with magnesium in ethanol-water mixtures to form a red complex having an absorption maximum at 490 nm in alkaline medium. A detailed study of the characteristics of this complex has been carried out and a spectrophotometric method for the determination of magnesium at the 0.4–4.0 μg ml^?1 level is proposed. The method has been sensitized by employing first derivative spectrophotometry. By the use of the derivative approach magnesium can be determined between 0.08–0.40 μg ml^?1. Statistical analysis of the results is also described.     

Determination of Morestan Residues in Water and Foodstuffs by Transmitted Room Temperature Solid Phase Spectrophosphorimetry

Abstract

A method for the determination of the pesticide morestan by means of transmitted room temperature solid phase spectrophosphorimetry has been developed. The method is based on the native phosphorescence showed by the morestan when it is fixed in a Whatman No 4 paper as a solid support. The excitation and emission wavelengths were 362 and 527 nm, respectively. The optimum phosphorescent emission was obtained when the delay time was 0.15 ms and the gate time 12.0 ms without need of a heavy atom. The linear dynamic range was between 0.1 and 1.0 μg.ml^?1, and the detection and quantification limits were 0.03 and 0.09 μg.ml^?1, respectively. The precision of the method, expressed as the relative standard deviation of ten samples at the 0.6 μg.ml^?1 concentration level, was 3.0%. The method was applied to the determination of the pesticide in different type of waters, potatoes and vegetables.     

Molecular emission cavity analysis: Part 23. Determination of Nitrite and Nitrate after Conversion to Nitrogen Monoxide

Molecular emission cavity analysis is applied to the determination of nitrite and nitrate after their reduction to nitrogen monoxide by iodide or zinc. The white emission stimulated from nitrogen monoxide in an oxy-cavity placed in a hydrogen—nitrogen diffusion flame is measured at 526 nm. Calibration graphs are linear up to 300 μg N ml^-1; the detection limit is 0.5 μg N ml^-1 for nitrite and 2 μg N ml^-1 for nitrate. There are few interferences. Procedures for the determination of nitrite and nitrate in admixture are described.     

Kinetic-Spectrophotometric Determination of Molybdenum(VI) Based on Its Catalytic Effect on the Thionine-Hydrazine Reaction

Abstract

A kinetic method for the determination of trace amounts of Mo(VI) (0.05-4 μg ml^?1) based on its catalytic effect on the reduction of thionine by hydrazine monochloride in strongly acidic media is reported. The reaction is monitored spectrophotometrically by measuring the decrease in absorbance of thionine at 605 nm after a fixed time (5 min.). The detection limit of the method is 23 ng ml^?1 and the relative standard deviation (RSD) for 0.05 μg ml^?1 of Mo(VI) is 1.2% (n=7). The method is almost free from interferences, especially from large amounts of tungsten. The procedure was successfully applied to the determination of trace amounts of molybdenum in steel.     

Rapid spectrophotometric determination of ruthenium(III) with prochlorperazine maleate

A rapid, simple spectrophotometric method for the determination of μg amounts of ruthenium, based on the formation of a pink complex between the metal and prochlorperazine maleate (PCPM) in sulphuric or hydrochloric acid solution, is described. The complex has an absorption maximum at 530 nm and its molar absorptivity is 6.733·10³ l mol^?1 cm^?1. The sensitivity is 0.0151 μg Ru cm^?2 for log I_o/I = 0.001. Beer's law is valid over the range 0.2–10 μg Ru ml^?1 ; the optimal range for spectrophotometric determination is 0.8–8.0 μg Ru ml^?1. Job's method of continuous variation, the mole ratio method and the slope ratio method indicate a 1:1 composition for the complex. The effects of acidity, time, temperature, order of addition of reagents, reagent concentration, and the interferences from various ions are reported.     

The determination of hydrazine and 1,1-dimethylhydrazine,separately or in mixtures,by high-pressure liquid chromatography

A rapid, sensitive liquid chromatographic method for the determination of hydrazine and 1,1-dimethylhydrazine, separately or in mixtures of varying proportions, is described. The procedure involves salicylaldehyde derivative formation followed by chromatography on a reversed phase (octadecylsilane) column with acetonitrile (52%)—0.14 M potassium dihydrogenphosphate (48%) as a mobile phase and u.v. (254 nm) detection. This system is sensitive to 2 μg ml^-1 of hydrazine and 5 μg ml^-1 of 1,1-dimethylhydrazine and has a relative standard deviation of less than 1%. Monomethylhydrazine forms an unstable salicylaldehyde hydrazone; although it cannot be determined, it can be detected (sensitivity 5 μg ml^-1 ) and does not interfere with quantitative measurement of either hydrazine or 1,1-dimethylhydrazine.     

Fluorimetric determination of ascorbic acid with o-phenylenediamine

A simple and sensitive fluorimetric method for the determination of ascorbic acid (AA) is described. The method is based on the condensation reaction between AA and o-phenylenediamine (OPDA) in the absence of the oxidant. The fluorescence intensity is measured at excitation and emission wavelengths of 360 and 430 nm, respectively. Under optimum condition, a linear relationship is obtained between the fluorescence intensity and the concentration of AA in the range of 0.05-40 μg ml⁻¹. The detection limit is 0.006 μg ml⁻¹, which is obviously lower than that of other fluorimetric methods reported.