Flow injection fluorometric determination of ascorbic acid using perylenebisimide-linked nitroxide

A simple and sensitive flow injection fluorometric method for the determination of ascorbic acid is described. Perylenebisimide-linked nitroxide (PBILN) is used as a fluorescent reagent, which permits the selective determination of ascorbic acid. The fluorescence of the perylenebisimide moiety in PBILN is quenched by the nitroxide moiety, which is linked to the perylenebisimide. When a stream of a solution of ascorbic acid is merged with a stream of PBILN, the ascorbic acid reacts with the nitroxide moiety of PBILN to form hydroxylamine, and the fluorescence properties of the perylenebisimide moiety are recovered. As a result, a peak-shaped fluorescence signal is produced, which can be observed by a fluorescence detector located downstream. Under optimized conditions, a good linear relationship between the concentration of ascorbic acid and peak height in the concentration range from 0.5 to 10 μmol L⁻¹ was found and the detection limit (S/N = 3) was 0.28 μmol L⁻¹. The relative standard deviation for the determination of 4.0 μmol L⁻¹ ascorbic acid samples was 1.0% (n = 5). The proposed method was applied to the determination of ascorbic acid in several soft drink beverages and the analytical results were in good agreement with those obtained using a conventional method.     

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).     

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 μg mL^?1, with a relative standard deviation of 1.6% (n = 11), a detection limit of 2.7 μg mL^?1 and a sample throughput of ¶60 samples h^?1. The photochemical method shows a linear range between 1 and 80 μg mL^?1, with a relative standard deviation of 1.0% (n = 11), a detection limit of 0.5 μg mL^?1 and a sample throughput of 40 samples h^?1.     

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.     

Stepwise injection photometric determination of ascorbic acid in drugs

A procedure is developed for the photometric determination of ascorbic acid in drug preparations. It is based on the rapid and highly selective reaction of ascorbic acid with a novel reagent, the guanidinium salt of 1-bismuto-11-molybdophosphoric heteropolyacid. The detection limit for ascorbic acid in stepwise injection analysis makes 15 mg/L, and the duration of single analysis, 5 min.     

流动注射化学发光法测定肉桂酸

碱性条件下,肉桂酸对Luminol-H2O2-纳米银化学发光体系有较强的增敏作用,据此,结合流动注射技术,建立了测定肉桂酸的新方法。该法线性范围为2.5×10-8～2.5×10-6mol/L,检出限为6.0×10-9mol/L,对1.0×10-7 mol/L的肉桂酸平行测定9次,相对标准偏差为2.5%。该法可用于尿液中肉桂酸的测定。     

Flow injection spectrophotometric or conductometric determination of ascorbic acid in a vitamin C tablet using permanganate or ammonia

Two simple flow injection (FI) procedures for the determination of ascorbic acid content in a vitamin C tablet are proposed: spectrophotometric involving injection into a stream of acidic potassium permanganate solution and monitoring its color change due to the redox reaction; FI conductometry based on the neutralization of ascorbic acid injected into a flowing ammonia solution yielding a change in conductivity. The procedures have been applied to the analysis of locally commercial vitamin C tablet samples. A through-put of at least 90 injections h⁻¹ can be achieved. The relative standard deviation was found to be 2.5% (for a 50 mg vitamin C tablet; n=7) for both. Results obtained by either procedure agree with a standard titrimetric method.     

Flow injection analysis methods for determination of diffusion coefficients

Two flow injection analyses (FIA) methods for the determination of diffusion coefficients in a straight single tube FIA system were developed. Based on the analytical solution of the convection-diffusion equation, linear relationships of the logarithmic values of the dispersion coefficient (D) and the half-peak width (W_1/2) with the diffusion coefficient (D_m) were obtained. Experiments were designed to verify these methods. For example, for potassium hexacyanoferrate (III) a D_m value of 0.72 × 10⁵ cm² s⁻¹ was found versus a literature value of 0.76 × 10⁵ cm² s⁻¹ (error, 5%). For potassium hexacyanoferrate (II) a D_m value of 0.67 × 10⁵ cm² s⁻¹ was obtained versus a literature value of 0.63 × 10⁵ cm² s⁻¹ (error, 6%). The diffusion coefficients of some important biomedical compounds, such as dopamine, epinephrine, norepinephrine and ascorbic acid, were then determined. The values of 10⁵ D_m/cm² s⁻¹ are 0.60 ± 0.03, 0.44 ± 0.02, 0.60 ± 0.01 and 0.68 ± 0.06, respectively.     

Individual and simultaneous determination of uric acid and ascorbic acid by flow injection analysis

Flow injection methods for the individual and simultaneous determination of ascorbic acid and uric acid are proposed. A spectrophotometer and a miniamperometric detector are connected in sequence. The calibration graphs for uric acid obtained by measuring its absorbance at 293 nm and its current at +0.6 V are linear up to at least 80 and 70 mug/ml, respectively, with an rsd (n = 10) of 1 % for both methods at mid-range concentrations. The calibration graph for ascorbic acid with amperometric detection is linear up to 80 mg/l. with an rsd (n = 10) of 0.8% at 30 mg/l. The simultaneous determination of uric acid and ascorbic acid is based on measurement of the absorbance of uric acid at 393 nm and amperometric determination of both analytes at +0.6 V. The average relative errors of the analysis of binary mixtures of uric acid and ascorbic acid are 2.2 and 4.2%, respectively.     

Sequential injection redox or acid-base titration for determination of ascorbic acid or acetic acid

Two sequential injection titration systems with spectrophotometric detection have been developed. The first system for determination of ascorbic acid was based on redox reaction between ascorbic acid and permanganate in an acidic medium and lead to a decrease in color intensity of permanganate, monitored at 525 nm. A linear dependence of peak area obtained with ascorbic acid concentration up to 1200 mg l⁻¹ was achieved. The relative standard deviation for 11 replicate determinations of 400 mg l⁻¹ ascorbic acid was 2.9%. The second system, for acetic acid determination, was based on acid–base titration of acetic acid with sodium hydroxide using phenolphthalein as an indicator. The decrease in color intensity of the indicator was proportional to the acid content. A linear calibration graph in the range of 2–8% w v⁻¹ of acetic acid with a relative standard deviation of 4.8% (5.0% w v⁻¹ acetic acid, n=11) was obtained. Sample throughputs of 60 h⁻¹ were achieved for both systems. The systems were successfully applied for the assays of ascorbic acid in vitamin C tablets and acetic acid content in vinegars, respectively.     

Flow injection amperometric detection of ascorbic acid using a Prussian Blue film-modified electrode

The PB film-modified electrode was used as an amperometric detector for flow injection analysis of ascorbic acid. The modified electrode detector showed good sensitivity, stability and reproducibility. The calibration curve for ascorbic acid was linear over the concentration range from 5.0x10(-6) to 1.0x10(-3) mol l(-1) with a slope of 19.9 mA mol(-1) per litre and a correlation coefficient of 0.999. The detection limit of this method was 2.49x10(-6) mol l(-1). The relative standard deviation of six replicate injections of 2.5x10(-4) mol l(-1) ascorbic acid was 2.5%. The results obtained for ascorbic acid determination in pharmaceutical products are in good agreement with those obtained by using the procedure involving the reaction between triiodide and ascorbic acid.     

Flow injection analysis of ascorbic acid at a methylene green chemically modified electrode

 In flow injection analysis (FIA) of ascorbic acid, methylene green (MG) modified carbon paste electrodes showed high catalytic activity and stability, reducing the oxidation overpotential by 400 mV. The linear response range was over 3 orders of magnitude and the detection limit was 1×10^-8 mol/L eq. 0.25 pmol with S/N=3. The influence of various experimental conditions was explored for optimum analytical performance. Received: 2 January 1996/Accepted: 23 January 1996     

Flow injection analysis of ascorbic acid at a methylene green chemically modified electrode

 In flow injection analysis (FIA) of ascorbic acid, methylene green (MG) modified carbon paste electrodes showed high catalytic activity and stability, reducing the oxidation overpotential by 400 mV. The linear response range was over 3 orders of magnitude and the detection limit was 1×10^-8 mol/L eq. 0.25 pmol with S/N=3. The influence of various experimental conditions was explored for optimum analytical performance. Received: 2 January 1996/Accepted: 23 January 1996     

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.     

Flow injection spectrophotometric determination of ultra trace amounts of oxalic acid

A new simple, sensitive and rapid catalytic-spectrophotometric method for the determination of oxalic acid has been described based on its catalytic effect on the redox reaction between dichromate and Brilliant cresyl blue in acidic media by means of a flow injection analysis method. The color change of Brilliant cresyl blue due to its oxidation was monitored spectrophotometrically at 625 nm. The calibration graph was linear in the range of 0.020-4.70 microg/mL oxalic acid with a limit of detection 0.005 microg/mL of oxalic acid. The relative standard deviation for ten replicate measurements of 0.020 microg/mL and 0.900 microg/mL was 2.2% and 1.7%, respectively. No serious interference was identified. Oxalic acid was determined in wastewater and in spinach by the proposed method with satisfactory results.     

Flow injection spectrophotometric determination of ultra trace amounts of oxalic acid

A new simple, sensitive and rapid catalytic-spectrophotometric method for the determination of oxalic acid has been described based on its catalytic effect on the redox reaction between dichromate and Brilliant cresyl blue in acidic media by means of a flow injection analysis method. The color change of Brilliant cresyl blue due to its oxidation was monitored spectrophotometrically at 625 nm. The calibration graph was linear in the range of 0.020–4.70 μg/mL oxalic acid with a limit of detection 0.005 μg/mL of oxalic acid. The relative standard deviation for ten replicate measurements of 0.020 μg/mL and 0.900 μg/mL was 2.2% and 1.7%, respectively. No serious interference was identified. Oxalic acid was determined in wastewater and in spinach by the proposed method with satisfactory results. Received: 28 October 1999 / Revised: 13 January 2000 / /Accepted: 20 January 2000     

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.