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1.
《Analytical letters》2012,45(10):2183-2191
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.  相似文献   

2.
Abstract

A new rapid, selective and sensitive method has been developed for the determination of maneb using pyrocatechol-violet(PV) as chelating reagent in the pH range of 7.5–11.0 in the presence of CTAB producing a complex which shows maximum absorption at 640 nm. Working range of the method is 0.2–3.0 μg ml?1 maneb (manganese ethylenebisdithiocarbamate). The molar absorptivity of the color system is 79600 1 mol?1 cm?1 and Sandell's sensitivity is 0.0033 μg cm?2. The reproducibility of the method has been checked by the 10 replicate analysis of 15 μg of maneb in 10 ml of solution. The method is quite sensitive and has been applied for the determination of maneb in various commercial samples, crops, grains and synthetic samples.  相似文献   

3.
《Analytical letters》2012,45(11):2045-2058
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.  相似文献   

4.
《Analytical letters》2012,45(6):603-611
Abstract

A new absorptiometric procedure for the determination of quintomycin sulphate in complex galenical mixtures is proposed, based on the reaction of the sample compound with a mineral acid-containing phloroglucinol solution. Absorbance readings at 448 nm obey Lambert-Beer's law within the concentration range from 4. 0 to 32. 0 μg ml?1. The method is operationally simple and has a good precision and an adequate selectivity.  相似文献   

5.
《Analytical letters》2012,45(11):2029-2043
Abstract

Two simple, rapid specific methods were developed for the determination of heptaminol and mexiletine and their dosage forms. The methods are based on the reaction of either heptaminol or mexiletine with acetylacetone-formaldehyde reagent to give a yellow chromophore measurable spectrophotometrically at 344 or 338 nm or flurometrically at 480 nm for heptaminol and mexiletine, respectively. The color was stable for at least 1/2 h. Beer's law was valid within a concentration range of 15–30 and 8–20 μg ml?1 spectrophotometrically and 0.2–0.8 and 0.4–1.0 μg ml?1 fluorometrically for heptaminol and mexiletine, respectively.  相似文献   

6.
《Analytical letters》2012,45(8):1575-1587
ABSTRACT

Four azo compounds based on diazotization of 2-aminobenzothiazole have been synthesized and characterized by elemental analysis as well as different spectroscopic techniques. The potentiality of the prepared compounds as new chromogenic reagents for the spectrophotometric determination of Mo6+ was studied by extensive investigation of optimum conditions favouring the formation of the coloured complexes. Beers law is obeyed in the concentration range 0.2-8.5 μg ml?1 whereas Ringbom optimum concentration range was 0.8-7.5 μg ml?1. The detection limit was 0.05 μg ml?1. The molar absorptivity and Sandell sensitivity of the formed complexes are calculated. The effect of interfering ions on the determination of Mo6+ was investigated. The relative standard deviations for six replicate determinations of 5.0 μg ml?1 of Mo6+ are 1.23, 1.47, 1.05 and 1.38 % using reagents I, II, III and IV, respectively. The proposed method has been applied to investigate the amount of Mo6+ in human urine samples. The molybdenum levels found between 0.5-2.1 μg/100 ml.  相似文献   

7.
《Analytical letters》2012,45(10):1875-1883
Abstract

A method is developed for the 2nd and 3rd order derivative spectrophotometric determination of 0.5–6 and 0.5–7 μ.ml?1 of ascorbic acid, respectively. For its determination in soft drinks a blank solution is prepared from the soft drink to be analyzed in order to avoid the interference from the other additives and colouring matter present.  相似文献   

8.
《Analytical letters》2012,45(10):1843-1856
Abstract

A simple and sensitive ultraviolet spectrophotometric method has been devised for the determination of amikacin, kanamycin, neomycin and streptomycin in pure form and in some pharmaceutical preparations. The method depends on the nitrosation of the primary amino groups followed by reaction with cyanoacetamide in ammonia medium at 100°C for 30 min, The reaction products exhibit a characteristic absorption. maximum at 270 nm. Beer's law is obeyed within the concentration ranges 4–40 μg ml?1 for amikacin, kanamycin and neomycin and 8–80 μg ml?1 for streptomycin with apparent molar absorptivities of about 1.85 × 104 for the first three compounds and 1.3×104 1. mole?1.cm?1 for streptomycin.  相似文献   

9.
《Analytical letters》2012,45(12):2279-2288
Abstract

An integrated-sensor method for the determination of formaldehyde based on retention of the reaction product of the analyte with p-rosaniline and sulfite in a flow-cell packed with Dowex 1-X-8 anion exchange resin was developed. The method has a good selectivity with a detection limit of 0.3 μg ml?1 (1 ml sample) or 75 ng ml?1 (2 ml sample), and a linear range between 1–30 μg ml?1. The relative standard deviations (n = 11) were 2.8 and 1.3% for 2 and 20 μg ml?1 formaldehyde, respectively. Depending on the working conditions, the sampling frenquency ranged between 10 and 18 h?1. The method was applied to the determination of formaldehyde in well water.  相似文献   

10.
《Analytical letters》2012,45(10):2223-2232
Abstract

A simple, sensitive and selective spectrophotometric method has been developed for the determination of thyroxine sodium. It is based on a reaction with excess of p-benzoquinone in ethanol (95%) whereby 1:1 (thyroxine sodium: quinone) coloured product is obtained, which has an apparent molar absorptivity of 2.911 × 103 1mol?1 and Beer's law is obeyed over the range of 40–200 μg.ml?1. When applied to tablets labelled to contain 100 μg, the proposed method gave mean recoveries of 99,13 ± 0.36% for different amounts of added authentic drug.  相似文献   

11.
《Analytical letters》2012,45(6):947-959
Abstract

A spectrophotometric method is described for the determination of Nicoumalone and Acebutolol hydrochloride based on the formation of molecular complex with the reduction product of Nicoumalone or hydrolysis product of Acebutolol hydrochloride and p-N-methyl benzoguinone monoimine [formed in situ from met01 (p-N-methylaminophenol sulfate) and potassium permanganate, PMBQMI] at pH 3.3. Quantitative measurements were made at the maximum absorption of 525 nm. Beer's law is obeyed in the range of 5–50 μg ml?1 and 5–60 μg ml?1 for Nicoumalone and Acebutolol hydrochloride respectively. The proposed method is comparable with the reference method when applied to pharmaceutical preparations, and tablets, An average percentage recovery of 99.5 ± 0.8 was obtained.  相似文献   

12.
《Analytical letters》2012,45(14):2708-2720
Abstract

A simple, sensitive, and direct spectrophotometric method has been developed for the assay of sparfloxacin in bulk and pharmaceutical preparations. The proposed method is based on the formation of ternary complex between an investigated drug, palladium(II) ion and eosin in the presence of methylcellulose as surfactant and acetate buffer of pH 4.2. Spectrophotometrically, under the optimum conditions, the ternary complex showed absorption maximum at 550 nm, with apparent molar absorptivity of 2.69×104 l mol?1 cm?1, Sandell's sensitivity of 0.01458 µg ml?1 and linearity in the concentration range 1.6–16 µg ml?1. The composition of the ternary complex was studied by Job's method of continuous variation and the result indicated that the molar ratio of SPFX: Pd: eosin is 1∶1∶1. The optimum reaction conditions and other analytical parameters are evaluated. The proposed method was successfully applied for the determination of SPFX in its pharmaceutical product with mean percentage recoveries of 99.71%. The observed data has been subjected to statistical analysis, which revealed high accuracy and precision.  相似文献   

13.
《Analytical letters》2012,45(13):2613-2623
ABSTRACT

A sensitive and selective spectrophotometric method has been developed for the determination of six phenothiazine neuroleptics. The method is based on the interaction of the drugs with chloramine-T in sulphuric acid medium to yield a red, reddish-violet, orange or greenish-blue intermediate with maximum absorption at 500-636 nm. Beer's law is obeyed over the range 5-125 μg ml?1 of the drugs. The apparent molar absorptivities were found to be in the range 1.04x103 to 5.46x103 1.mol?1cm?1. The investigated drugs were assayed in tablets and injections. The mean percentage recoveries were 97.65-101.75 and the relative standard deviations were found to be less than 2%.  相似文献   

14.
《Analytical letters》2012,45(1):169-182
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.  相似文献   

15.
《Analytical letters》2012,45(11):1905-1916
Abstract

A method is proposed for the simultaneous determination of mercury(II) and palladium(II) by first-derivative spectrophotometry based on the absorption spectra of their complexes with 5-(3,4-Methoxyhydroxyphenylmethylene)-2-thioxo-1,3-thiazolidine [5-(3,4-methoxyhydroxybenzylidene) rhodanine]. Zero-crossing measurement technique is found suitable for the measurement of the first-derivative value at the specified wavelengths. Mercury(II) (0.4-1.4 μg ml?1) and palladium(II) (0.08 - 1.8 μg ml?1) in different ratios have been determined simultaneously. A critical evaluation of the proposed method is performed by statistical analysis of the experimental data.  相似文献   

16.
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.  相似文献   

17.
《Analytical letters》2012,45(13):2595-2602
ABSTRACT

A derivative spectrophotometry was developed to determine miconazole in cream formulations that contain benzoic acid as preservative. The procedure was based on the linear relationship in the range 100-500 μg ml?1 between the drug concentration and the second derivative amplitudes at 276 nm. Results of the recovery experiments performed on various amounts of benzoic acid and of the determination of miconazole in cream confirmed the applicability of the proposed method to complex formulations.  相似文献   

18.
《Analytical letters》2012,45(10):1989-1998
Abstract

A sensitive and selective spectrophotometric flow injection analysis (FIA) method with chlorophosphonazo-mN has been developed for the determination of uranium(VI) in standard ore samples. Most of interfering ions are effectively eliminated by the masking reagent of diethylenetriaminepentaacetic acid (DTPA). In the U(VI)-chlorophosphonazo-mN system, the maximum absorption wavelength is at 680 nm and Beer's law is obeyed in the range of 1 to 15 μg ml?1. The correlation coefficient of the calibration curve is 0.9998, the sampling frenquency is 60 h?1, and the detection limit for uranium(VI) is 0.5 μg ml?1. The composition of the U(VI)-chlorophosphonazo-nN complex was established to be 1:2 by flow-through spectrophotometric and conventional molar ratios methods.  相似文献   

19.
《Analytical letters》2012,45(11):2455-2471
Abstract

A method is proposed for the simultaneous determination of nickel and manganese by first-derivative spectrophotometry based on their reactions with 2-(2-pyridylmethyleneamino)phenol (PMAP) Schiff base. The method allows the determination of Ni and Mn in the concentration range 0.3–3.0 μg ml?1 in mixtures with their ten-fold concentration ratio. The method has been applied for Ni and Mn determination in bronzes. To optimize the experimental conditions for spectrophotometric determination of Mn with PMAP stability constants at different pH values have been determined. A critical evaluation of the proposed method was performed by statistical analysis of the experimental data.  相似文献   

20.
《Analytical letters》2012,45(8):1511-1524
Abstract

Two methods have been developed for the simultaneous determination of Amitryptiline and Perphenazine: the zero-crossing (I) and the derivative ratio spectrum (II) methods and both use the derivative spectrophotometry.

The methods have been applicable in the ranges of 1 to 30 μg·ml?1 of Amitryptiline (I and II) and between 1 and 8 μg·ml?1 and from 1 to 7 μg·ml?1 of Perphenazine for the methods I and II respectively. The accuracy of the proposed methods have been studied and they have been used in the determination of Amitryptiline and Perphenazine in commercially available pharmaceuticals.  相似文献   

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