Kinetic spectrofluorimetric determination of trace ascorbic acid based on its inhibition on the oxidation of pyronine Y by nitrite

A highly sensitive spectrofluorimetric method is proposed for the determination of trace amount of ascorbic acid using a new indication. The method is based on the inhibition of ascorbic acid on the oxidation of pyronine Y (PRY) by nitrite. The detection limit for ascorbic acid is 0.012 microg ml(-1), the linear range of the determination is 0.02-0.36 microg ml(-1). Analytical parameters, such as reagent concentration, pH, reaction temperature and time, were optimized. The relative standard deviations of eleven replication determinations of 0.12 and 0.24 microg ml(-1) ascorbic acid were 1.4 and 0.72%, respectively. This method has been used to determine ascorbic acid in pharmaceuticals, vegetables, fruits and soft drink with satisfactory results.     

Determination of ascorbic acid in soft drinks, preserved fruit juices and pharmaceuticals by flow injection spectrophotometry: Matrix absorbance correction by treatment with sodium hydroxide

Two flow injection systems for the spectrophotometric determination of ascorbic acid at 245 nm have been described. On treatment with sodium hydroxide a fraction of the ascorbic acid was decomposed into substances, which do not absorb in UV region, and the decrease in signal measured. This was directly related to the amount of ascorbic acid present. The calibration graph was linear over the range 1-25 and 1-50 microg/ml in the two methods with a correlation coefficient of 0.9981 and 0.9994, respectively. The detection limit (2sigma) was 0.5 and 0.2 microg/ml, respectively. The RSD for 1 microg/ml standard was 2.5 and 1.8% (n = 6) in the two methods, and the sampling throughput 30/hr. The methods permitted the use of 6 microg/ml of 2-mercaptoethanol as an anti-oxidant and stabilizer for ascorbic acid, which is difficult to handle at its microg/ml level. Upon matrix absorbance correction, spiked samples that are known to contain UV-absorbing substances produced an average recovery of 101% with a RSD of 1.2%. The methods were used for the rapid and simple determination of ascorbic acid in soft drinks, preserved fruit juices and pharmaceuticals and the results thus produced compared with those obtained by previously checked methods involving titration with iodine, chloranil 2,6-dichlorophenolindophenol, and HPLC. When there was a disagreement between the results, this was traced to the presence of substances which are known to interfere in comparison methods.     

Kinetic method for determination of ascorbic acid on flow injection system by using its catalytic effect on the complexation reaction of an ultra sensitive colorimetric reagent of porphyrin with Cu(II)

A kinetic method performed on a flow injection system is described for the determination of ascorbic acid by using its catalytic effect on the complexation reaction of Cu(II) with 5,10,15,20-tetrakis(4-N-trimethyl-aminophenyl)porphyrin. The characteristic spectrum of porphyrin (Soret band), which shows intense absorption around 400 nm (epsilon>2.0 x 10(5) cm(-1)M(-1)), was used first time for determining ascorbic acid. By incorporating the complexation reaction into a flow injection system, ascorbic acid could be determined either over a broad dynamic range of 0.1-1000 microg/ml or at a trace level below 5 ng/ml. Good repeatability was also achieved by testing a working standard of 0.1 microg/ml with 10 injections at a throughput of 35 h(-1), obtaining a relative standard deviation of 0.11%. Substances like amino acids, vitamins, sugars, organic acids and metal ions, showed no or little interference even present at high concentrations. The method was validated in the determination of ascorbic acid contents of some commercially available soft drinks by comparison with the official 2,6-dichloroindophenol method with reasonable agreement.     

Kinetic spectrophotometric determination of ascorbic acid by reduction of toluidine blue

A simple kinetic method is described for the determination of ascorbic acid. The procedure is based on the reduction of toluidine blue with ascorbic acid. The rate of reaction is followed by measuring the decrease in absorbance of toluidine blue (lambda(max) = 600 nm) as a result of its decolorization upon reduction by ascorbic acid. Ascorbic acid in the range of 3-35 microg/ml was determined using slope and fixed time methods of analysis, while the variable time method allowed the determination of 5-50 microg/ml of ascorbic acid. The percent relative standard deviation of the method varied from 0.78 to 1.32% depending on the kinetic method used. The high sensitivity of the method also allows determination of low levels of ascorbic acid in some fruits and vegetables such as dew melon, water melon, parsley and coriander.     

Spectrophotometric method for the determination of ascorbic acid with iron (III)-1,10-phenanthroline after preconcentration on an organic solvent-soluble membrane filter

A solvent-soluble membrane filter is proposed for the simple and rapid preconcentration and spectrophotometric determination of ascorbic acid based on the reduction of 1, 10-phenanthroline (phen)-iron (III), which is collected on a nitrocellulose membrane filter as an ion-associate of the cationic complex of tri,phen-iron (II) [ferroin, Fe(phen)(2+)(3)] with an anionic surfactant (of dodecyl sulfate). The ion-associate collected is dissolved in a small volume of 2-methoxyethanol together with the filter. The colour intensity is measured at 510 nm against the reagent blank and is proportional to the content of ascorbic acid in the range 2.5-50 microg ascorbic acid in 5 ml of solvent with excellent reproducibility (RSD 3.2% for 200 microg 1(-1) ascorbic acid), the enrichment factor achieves 100-fold and detection limits better than 2.0 microg 1(-1) can be obtained. Diverse components of organic and inorganic compounds normally present in fruits, vegetable, beverages and urine do not interfere. The recoveries of the ascorbic acid added to the samples are quantitative.     

Flow injection kinetic spectrophotometric determination of ascorbic acid based on an inhibiting effect

A rapid and sensitive flow-injection kinetic spectrophotometric method is proposed for the determination of ascorbic acid. The procedure is based on the inhibiting effect of ascorbic acid on the enhancing effect of oxalate on the potassium dichromate-potassium iodide/rhodamine 6G system. The detection limit and linear ranges are 0.08 and 0.10-4.00 microg/ml, respectively. The relative standard deviation of 11 replicate measurements is less than 2.0%. This method has been successfully used to determine ascorbic acid in pharmaceuticals, tomatoes and oranges.     

Indirect spectrophotometric determination of ascorbic acid with ferrozine by flow-injection analysis

A FIA indirect spectrophotometric determination of ascorbic acid was developed using its reducing action on Fe(III) in acidic medium and following the spectrophotometric determination of the reduced iron by using sodium 3-(2-pyridyl)-5,6-diphenyl-1,2,4-triazine-4',4'-disulphonate (ferrozine) as chromogenic reagent in buffered medium (pH 5.5) and monitoring the absorbance signal at 562 nm. A three-line manifold with two reaction coils was used: in the first reaction coil, ascorbic acid reduces Fe(III) to Fe(II); and in the second one, the complexation reaction is developed. The linear range of the method was 0.5-10 mug ml(-1) of ascorbic acid, the detection limit being 0.028 mug ml(-1). The proposed method was sensitive, rapid (sampling rate of 90 samples h(-1)) and reproducible (RSD 0.19%, n=10). Satisfactory results were obtained in the determination of ascorbic acid in pharmaceutical preparations, fruit juices and urine testifying the applicability of the method to real samples.     

Selective spectrophotometric determination of ascorbic acid in drugs and foods

A new analytical method was developed for the determination of ascorbic acid. The method is based on the reaction of ascorbic acid with 4-chloro-7-nitrobenzofurazane (NBD-Cl) in the presence of 0.2M sodium hydroxide, where a bluish green colour (lambda(max) 582 nm) is developed after dilution with 50% (v/v) aqueous acetone solution. Beer's law was obeyed in a concentration range of 5-20 microg ascorbic acid/ml with a good correlation coefficient (r = 0.9990). The method was found to be highly specific for the determination of ascorbic acid in the presence of dehydro-ascorbic acid, all other vitamins and minerals possibly present in multivitamin preparations, rutin, salicylamide, acetyl salicylic acid, paracetamol, caffeine, phenylephrine hydrochloride and dipyrone. Moreover, the proposed procedure was also successfully applied for the determination of ascorbic acid in some canned and fresh fruit juices, some vegetables and infant milk products without interference from coloured and other substances present in the plant extracts.     

Spectrophotometric determination of ascorbic acid in pharmaceuticals by background correction and flow injection

Background correction has been shown to be an effective and indispensable modification in the spectrophotometric determination of ascorbic acid. The decomposition of ascorbic acid in pharmaceutical samples was carried out by incubation with sodium hydroxide to give products that were insensitive to ultraviolet light. The rapid oxidation in air of ascorbic acid, especially in dilute solutions, was avoided by the use of the flow injection principle for spectrophotometric determination and by employing a carrier stream of an anti-oxidizing nature consisting of 6 micrograms ml(-1) of 2-mercaptoethanol in 0.25% sulphuric acid. The optimized method with a single channel manifold made use of a carrier stream flow rate of 1.1 ml min(-1), an injection volume of 50 microl, a delay coil of 50 cm (0.5 mm i.d.) and detection at 245 nm. The throughput was at least 180 injections h(-1). The proposed flow injection method yielded results for the analysis of 0-20 micrograms ml(-1) of ascorbic acid that were 99-102% (relative standard deviation 0.6% or better) in agreement with those produced by comparable methods involving titration with iodine, chloranil or 2,6-dichlorophenolindophenol [4-(2,6-dichloro-4-hydroxyphenylimino)cyclohexa-2,5-dieno ne], and high-performance liquid chromatography. When the agreement was not good (as low as 14% with respect to the method being compared), this was traced to the presence of substances which are known to interfere in one or other of the methods of comparison.     

Optimization of a chemical modifier in the determination of selenium by graphite furnace atomic absorption spectrometry and its application to wheat and wheat flour analysis.

A method for the determination of total selenium in wheat and wheat flour using graphite furnace atomic absorption spectrometry (GFAAS) with palladium/ascorbic acid as a chemical modifier was studied. The effects of nickel nitrate, palladium/ascorbic acid, and palladium/magnesium nitrate as chemical modifiers on the sensitivity in the determination of selenite, selenate and selenomethionine by GFAAS were compared. The palladium/ascorbic acid modifier was used for the determination of total selenium in wheat and wheat flour, because the oxidation states of the selenium ion are not important in the determination. The detection limit was estimated to be 1 microg L(-1) (calculated as 3sigma of the blank); the calibration curve was linear for the concentration range 5 - 50 microg L(-1) and the recovery range was 96.66 - 101.80%. The optimal ashing and atomizing temperatures were 1300 degrees C and 2250 degrees C, respectively. The proposed method was successfully applied to the determination of total selenium in wheat and wheat flour.     

Catalytic-kinetic determination of trace amount of formaldehyde by the spectrophotometric method with a bromate-Janus green system

A new simple and rapid catalytic kinetic method for the determination of trace amount of formaldehyde is described. The method is based on the catalytic effect of formaldehyde on the oxidation of Janus green by bromate in the present of sulfuric acid. The reaction monitored spectrophotometrically by measuring the decrease in absorbance of the reaction mixture at 618 nm. The fixed-time method was used for the first 150 s. For initiation of the reaction, under the optimum conditions, in the concentration range of 0.003-2.5 microg ml(-1) formaldehyde can be determined with a limit of detection 0.0015 microg ml(-1). The relative standard deviation of five replicate measurements is 2.3% for 1.0 microg ml(-1) of formaldehyde. The method was used for the determination of formaldehyde in real samples with satisfactory results.     

Sensitive kinetic-spectrophotometric determination of iodate in iodized table salt based on its accelerating effect on the reaction of bromate with chloride ion in the presence of hydrazine.

A simple, precise, sensitive and accurate method was developed for rapid determination of trace quantities of iodate. The method is based on the accelerating effect of iodate on the reaction of bromate and chloride acid in the presence of hydrazine in acidic media. The decolorization of Methyl Orange with the reaction products was used to monitor the reaction spectrophotometrically at 525 nm. Iodate could be determined in the concentration ranges of 0.03 - 1.2 microg ml(-1). The relative standard deviation for ten replicate determinations of 0.3 microg ml(-1) of iodate was 1.65%. The proposed method was applied to the determination of iodate in table salts with satisfactory results.     

Spectrophotometric determination of urea in dermatologic formulations and cosmetics

A rapid, relatively sensitive, and low-cost method for the determination of water-soluble urea content in dermatological therapy products and cosmetics is proposed using a new spectrophotometric assay with water as the only extraction solvent. Spectrophotometric methods involve addition of a known excess of bromate to urea in an acid medium, followed by the determination of residual bromine and chlorine reacting with methyl orange and measurement of absorbance at 505 nm. The absorbance increases linearly with urea concentration (r = 0.9998). The systems obey Beer's law for 6 - 90 microg ml(-1). The calculated apparent molar absorbance values are found to be 4.537 x 10(3) dm(3) mol(-1) cm(-1) and the Sandell's sensitivity is 0.013 microg cm(-2). The variables affecting the rate of the reaction were investigated. The relative standard deviation for five-replication determination of 60 microg ml(-1) urea was 2.1% and the detection limit of the method is 0.34 ng ml(-1).     

Flow injection spectrophotometric determination of ascorbic acid in soft drinks and beer

Two spectrophotometric methods, a photochemical and a non-photochemical, for the determination of ascorbic acid in soft drinks and beer using a flow-injection system are proposed. The non-photochemical method is based on the redox reaction that takes place between ascorbic acid and Fe(III), yielding dehydroascorbic acid and Fe(II). Fe(II) reacts with 1,10-phenantroline, originating the reddish orange Fe(phen)3(2+) complex (ferroin). This complex is spectrophotometrically monitored at 512 nm, and the signal is directly related to the concentration of ascorbic acid in the sample. The photochemical method has the same basis, nevertheless, uses the irradiation with visible light to enhance the redox reaction and so achieve higher sensitivities in the analysis. The non-photochemical method shows a linear range between 5 and 80 microg mL(-1), with a relative standard deviation of 1.6% (n = 11), a detection limit of 2.7 microg mL(-1) and a sample throughput of 60 samples h(-1). The photochemical method shows a linear range between 1 and 80 microg mL(-1), with a relative standard deviation of 1.0% (n = 11 ), a detection limit of 0.5 microg mL(-1) and a sample throughput of 40 samples h(-1).     

Kinetic spectrophotometric method for the determination of oxalic acid by its catalytic effect on the oxidation of safranine by dichromate

A new catalytic kinetic spectrophotometric method for the determination of oxalic acid has been described based on its catalytic effect on the redox reaction between safranine and dichromate in dilute sulfuric acid media. The reaction is monitored photometrically by measuring the decrease in absorbance of safranine at the maximum wavelength of 530 nm. Under the optimum conditions, a calibration graph from 0.10 to 10.00 microg ml(-1) of oxalic acid with a detection limit of 0.08 microg ml(-1) was obtained. The relative standard deviation (R.S.D.) for ten replicate measurements of 1.0 and 5.0 microg ml(-1) oxalic acid was 2.7 and 2.5%, respectively. The purposed method is simple, sensitive, selective and inexpensive. The applicability of the proposed method was determined by the determination of oxalic acid in spinach and wastewater samples with satisfactory results.     

Rapid determination of chromium(VI) in electroplating waste water by use of a spectrophotometric flow injection system

A new rapid and sensitive FI method is reported for spectrophotometric determination of trace chromium(VI) in electroplating waste water. The method is based on the reaction of Cr(VI) with sodium diphenylamine sulfonate (DPH) in acidic medium to form a purple complex (lambda(max) = 550 nm). Under the optimized conditions, the calibration curve is linear in the range 0.04-3.8 microg ml(-1) at a sampling rate of 30 h(-1). The detection limit of the method is 0.0217 microg ml(-1), and the relative standard deviation is 1.1% for eight determinations of 2 microg ml(-1) Cr(VI). The proposed method was applied to the determination of chromium in electroplating waste water with satisfactory results.     

Elimination of the interferences of anions in the kinetic spectrophotometric determination of vanadium (V) solution

Accurate determination of vanadium (V) in industrial waste water is of great importance in environmental, biological and toxicological studies. Most of kinetic spectrophotometric methods based on the catalytic effect of vanadium (V), when applied to real samples for determination of trace levels of vanadium (V) lack the satisfactory sensitivity and selectivity. This may be attributed to the serious interferences of various anions which are common pollutants in industrial waste water. The oxidation of gallic acid by ammonium persulphate, catalysed by vanadium (V) was chosen for our study. The effect of the serious interferences of various anions such as chloride, bromate, bromide, chromate, iodide, iodate, molybdate, carbonate and sulphate on the net absorbance given by 4 microg l(-1) of vanadium (V) solution were studied. The minimum concentrations of citric acid, EDTA, ascorbic acid and oxalic acid as leveling off agents required to level off interfering effects due to the aforementioned anions in the kinetic determination of vanadium (V) were 50, 70, 80 and 120 microg ml(-1), respectively. In the presence of optimum concentrations of effective leveling off agents, the dynamic range can be extended and sensitivity increased as compared with the proposed method without levelling off agents. The proposed method is a rapid, sensitive and selective method for the determination of ultra trace amounts of vanadium (V) in real samples with satisfactory results.     

Spectrophotometric determination of uranium using ascorbic acid as a chromogenic reagent

A spectrophotometric method has been developed for the determination of uranium(VI) using ascorbic acid. Uranium in the hexavalent state forms a reddish-brown coloured complex with ascorbic acid. The colour intensity of the complex is maximum at pH 4.2-4.5 and is stable for 24 hr. The absorbances of uranium(VI)-ascorbic acid complex at 360 and 450 nm are used for its quantification. Uranium in the range 8-200 microg/ml has been determined with good precision. The method allows the determination of uranium in the presence of many metal ions present as impurities. The described method is simple, accurate and applicable to uranium concentration relevant to the PUREX process and thus can be used for analytical control purposes.     

Determination of tributyltin in toluene extract from sea water by graphite furnace atomic absorption spectrometry with a new matrix modifier

A new matrix modifier composed of calcium and chromium[VI] was proposed for the determination of tributyltin (TBT) in toluene extract from sea water containing sediment by graphite furnace atomic absorption spectrometry (GFAAS). Fourteen inorganic and organic compounds (barium, calcium, chromium[VI], lanthanum, magnesium, nickel, palladium, strontium, calcium-chromium[VI], calcium-strontium, nickel isocaprylate, 5%-, 10%-aqueous solution of ascorbic acid and toluene-saturated solution of ascorbic acid) as a matrix modifier were comparatively studied and a matrix modifier composed from 5 microg of calcium and 1 microg of chromium[VI] was found to give the best performance. The interference effects of co-existing elements in sea water containing sediment (aluminium, iron, magnesium, sodium and strontium) were studied. TBT in eight toluene extracts was determined by GFAAS with the proposed matrix modifier. The relative standard deviation was 3.0% for 63 ng ml(-1) of TBT (n = 11). The recoveries were 88-104%. The characteristic mass was 7 pg. The linearity range was 0-250 ng mg(-1).     

Spectrophotometric determination of iron with ferrozine by flow-injection analysis

Two methods for the determination of iron by normal FIA and reversed FIA were developed using sodium 3-(2-pyridyl)-5,6-diphenyl-1,2,4-triazine-4',4'-disulphonate (ferrozine). The reagent formed a chelate with Fe(II) in hexamethylentetramine buffered medium at pH 5.5. In one previous reaction coil Fe(III) was reduced to Fe(II) by ascorbic acid and in the other reaction coil the complexation reaction was developed. The linear range of the determination was 0.5-6 and 0.1-5 mug ml(-1) of iron for normal FIA and reversed FIA respectively. The proposed method was sensitive (detection limit 0.012 and 0.010 mug ml(-1)), rapid and reproducible (RSD 0.3 and 0.28%). The method was satisfactorily applied to the determination of iron in waste water, toadstool tissue, potato leaves, human hair and bauxites at a sampling rate of 90 and 50 samples h(-1) for normal FIA and reversed FIA respectively.