Flow injection determination of formaldehyde by its catalytic effect on the oxidation of sulfonazo III by bromate with spectrophotometric detection.

A simple and sensitive flow injection method with spectrophotometric detection was developed for the determination of formaldehyde. The method is based on the catalytic effect of formaldehyde on the oxidation of sulfonazo III with bromate in acidic media. The decrease in absorbance of the reaction mixture was measured at 566 nm. The calibration graph was linear in the range of 0.005 to 2.80 microg ml(-1) formaldehyde at a rate of 38 +/- 4 samples h(-1). The limit of detection was 4 ng ml(-1). The relative standard deviations for ten replicate measurements of 0.20, 0.50 and 1.00 microg ml(-1) formaldehyde were 1.3, 0.8 and 0.7%, respectively. The method was applied to the determination of formaldehyde in river water, shampoo and melamine-formaldehyde resin.     

Determination of trace formaldehyde in blood plasma by resonance fluorescence technology

A novel method for the determination of trace formaldehyde in blood plasma has been established by using resonance fluorimetry technique. It was based on the fact that oxidation of pyronine Y by potassium bromate was catalyzed by formaldehyde in sulfuric acid. When the wavelength interval was at Δλ = 0 nm, it was found that the decreased intensity (ΔF) of resonance fluorescence at 574.6 nm was proportional to the concentration of formaldehyde in the range of 1.27 × 10⁻² to 2.28 μg mL⁻¹. The limit of detection and the average recovery for formaldehyde were 3.80 ng mL⁻¹ and 101.6% (n = 6), respectively. The present method had been applied to the determination of trace formaldehyde in blood plasma, and the obtained results were in good agreement with those obtained by the resonance light scattering method.     

Spectrophotometric determination of formaldehyde by using formaldehyde dehydrogenase

A new method for the determination of formaldehyde by using formaldehyde dehydrogenase is described. The method is based on the quantitative oxidation of formaldehyde with oxidized nicotinamide adenine dinucleotide (NAD⁺), in the presence of formaldehyde dehydrogenase, to form the reduced dinucleotide (NADH). This enzyme does not require glutathione as a co-factor and the NADH produced, which is directly proportional to the concentration of formaldehyde in the assay solution, is then measured spectrophotometrically at 340 nm. Formaldehyde can be determined in the range 0.3–8.0 μg ml^?1 (1.0×10^?5–2.7× 10^?4 M) with a sensitivity of 0.216 absorbance/ μg ml^?1 (0.0065 absorbance/μM). Optimal conditions and the selectivity of this enzyme toward formaldehyde are described.     

Microwave-assisted on-line derivatization for sensitive flow injection fluorometric determination of formaldehyde in some foods

A rapid and sensitive flow injection fluorometry has been developed for the determination of formaldehyde based on the microwave on-line accelerating its Hantzsch reaction with cyclohexane-1,3-dione. Under the optimized conditions, the fluorescent intensity is proportional to formaldehyde content in the range from 0.05 ng/mL to 2.000 μg/mL. The detection limit (S/N = 3) is 0.02 ng/mL and the analytical frequency is 28 injections per hour. The relative standard deviations are 2.2% and 3.1% for eleven injections of 0.100 and 0.001 μg/mL of formaldehyde, respectively. With the assistance of microwave irradiation, a best sensitive fluorometry was established for the determination of formaldehyde at a high analytical frequency. This method was successfully applied to food analysis without requiring any sample pretreatment, and the determination results were correlated well with those obtained by the standard method with a sample pretreatment of steam distillation.     

Determination of selenium in blood plasma and serum by flow injection hydride generation atomic absorption spectrometry

A flow injection hydride generation atomic absorption spectrometric (AAS) method has been used to determine the selenium concentrations of human serum and plasma samples following digestion with nitric, sulphuric and perchloric acids. In the hydride generation process, reduction was carried out by sodium tetrahydroborate to produce a hydride that was atomized in a flame-heated atomisation cell. The method had a detection limit of 1.2 ng ml-1 and a sensitivity of 2.1 ng ml-1. Within-run precisions of 5.8% at 20 ng ml-1 and 4.5% at 80 ng ml-1, and between-run precisions of 4.8% at 69 ng ml-1 and 3.4% at 80 ng ml-1 were obtained. An inter-laboratory comparison study with a graphite furnace AAS method was carried out and the results showed excellent agreement. The flow injection method of sample introduction allowed the use of a sample volume of 330 microliters with an injection rate of 90 injections per hour.     

Spectrophotometric determination of traces of formic acid and formaldehyde in effluent waters with or without preconcentration

Formic acid plus formaldehyde are determined after reducing the acid with nascent hydrogen; formaldehyde alone is determined without reduction. The chromotropic acid method is used in 6–7.5 M sulfuric acid. The limit of determination is 0.05 μg ml^-1 without preconcentration and 0.05 ng ml^-1 with preconcentration by extraction with diethyl ether. Analysis time is 30 min by the direct method and 1 h with preconcentration.     

Pharmacokinetics of clenbuterol in the ostrich.

The aim of this study was to investigate the pharmacokinetics of clenbuterol in the ostrich as no such data is available. Clenbuterol (2 mg) was given as a single oral dose to nine ostriches. Blood samples were collected over a period of 96 h after administration and urine for a period of 5 d. Plasma and urine samples were frozen at -20 degrees C pending analysis. Clenbuterol was quantified using a gas chromatograph-mass selective detector. The method for quantification of clenbuterol in plasma was validated by analysing spiked quality control samples at different concentrations. The limit of quantification was determined to be 0.75 ng ml-1 with an absolute recovery of more than 80%. The geometric mean maximum plasma clenbuterol concentration was 4.40 ng ml-1 with 3.0 h as the median time for maximum concentration. The plasma elimination half-life was 19.7 h. The clenbuterol concentration was above 0.75 ng ml-1 in plasma for 48 h and above 1.0 ng ml-1 in urine for 5 d. These data can be useful in residue analysis for clenbuterol in ostriches.     

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.     

Spectrophotometric determination of formaldehyde

A new spectrophotometric method for the determination of micro amounts of formaldehyde in aqueous and methanol solutions is based on the oxidation of formaldehyde by hydrous silver oxide at pH 11-12.5 and oxidation of the metallic silver produced, with iron(III) in the presence of Ferrozine. The absorbance of the resulting iron(II)-Ferrozine complex at 562 nm is proportional to the amount of formaldehyde and corresponds to an apparent molar absorptivity of 5.58 x 10(4) 1.mole(-1).cm(-1).     

Sensitive determination of paraquat and diquat at the sub-ng ml-1 level by continuous amperometric flow methods.

Two methodologies are described for the determination of paraquat and diquat. The first is based on the pre-treatment of an electrode with a surfactant solution, which improves the electrochemical determination of the herbicides. Linear calibration graphs were obtained in the ranges 10-80 and 10-100 ng ml-1 for paraquat and diquat, respectively. The limits of detection were 6.32 for paraquat and 4.80 ng ml-1 for diquat. The method was applied to the determination of the herbicides in synthetic water samples. The second methodology is based on the preconcentration of paraquat and diquat in a minicolumn packed with a cation-exchange material. The determination ranges and detection limits depend on the sample volume used (5-50 ml). Thus, 50 ml of sample provides limits of detection of 0.016 and 0.020 ng ml-1 for paraquat and diquat, respectively. The applicability of the method was demonstrated with the determination of the herbicides in both synthetic and real water samples.     

Spectrofluorimetric determination of formaldehyde in air after collection onto silica cartridges coated with Fluoral P

In the present work, a sensitive and selective fluorimetric method for formaldehyde determination in air samples is described. The method is based in the reaction between formaldehyde and Fluoral P producing 3,5-diacetyl-1,4-dihydrolutidine, which, when excited at 410 nm, emits fluorescence at 510 nm.The Fluoral P was prepared by the reaction of 0.3 ml of acetic acid, 0.2 ml of acetylacetone and 15.4 g of ammonium acetate. Then, the volume was completed to 100 ml with deionized water. The Fluoral P obtained, if stored under refrigeration in the dark, can be used, safely, for 60 days.The calibration curve obtained with concentrations of formaldehyde in the range of 12 to 192 ng ml⁻¹ (n=9) was Intensity=1.11C+0.06 (R²=0.9920). In the quantification of formaldehyde, air samples were passed at 1 l min⁻¹, during 120 min, through glass impingers containing 40 ml of Fluoral P, followed by direct fluorescence measuring, or through two SEP PAK silica cartridges, coated with Fluoral P. The cartridges were eluted with 10 ml of Fluoral P solution and quantified by spectrofluorimetry. Under these conditions, the detection limit (S/N=3) obtained was 2.0 ng ml⁻¹.The new methodology was validated by comparison with a well-known HPLC method in which formaldehyde was collected into SEP PAK C18 cartridges coated with 2,4 dinitrophenylhydrazine. The application of the t_95% test did not show significant differences between the HPLC and either fluorimetric methodologies.This method has been used in the determination of gas phase formaldehyde in both indoor and outdoor sites. For the indoor site, the measured concentrations were in the range of 9.0 to 67.7 μl l⁻¹, while for the outdoor site they were in the range of 16.8 to 38.8 μl l⁻¹. Further, due to the ease of handling in field studies, the SEP PAK cartridges coated with Fluoral P were used. The formaldehyde concentrations thus determined, in outdoor sites, were in the range of 2.09 to 25.1 μl l⁻¹. The main advantage of this analytical procedure is its selectivity for formaldehyde, without interferences from bisulfite and other aldehydes, especially acetaldehyde, and low blank level, resulting in low detection limits. In addition, very little sample preparation is required.     

Kinetic spectrophotometric method for rapid determination of trace formaldehyde in foods

A simple and sensitive kinetic-spectrophotometric method was developed for the determination of ultra trace amount of formaldehyde in food samples. The method was based on the oxidation of rhodamine B (RhB) by potassium bromate in sulfuric acid medium (formaldehyde as catalyst). The reaction was monitored by measuring the decrease in absorbance of the dye at 515 nm after 6 min. The developed method allowed the determination of formaldehyde in the range of 10–100 μg L⁻¹ with good precision, accuracy and the detection limit was down to 2.90 μg L⁻¹. The relative standard deviations for the determination of 10 and 60 μg L⁻¹ of formaldehyde were 3.0% and 1.9% (n = 10), respectively. The method was found to be sensitive, selective and was applied to the determination of formaldehyde in foods with satisfactory results.     

Differential-pulse voltammetric determination of trace formaldehyde using magnetic microspheres and magnetic electrode

A new type of magnetic polymer microsphere containing acylhydrazine groups on the surface was synthesized. They can be reacted with formaldehyde to produce an electroactive adduct. Reduction of these derivatives following aggregation on a magnetic electrode is possible and is effective in the indirect determination of formaldehyde. The experimental conditions and electrode structure are discussed. Under the optimum conditions, it was found that the peak potential (Ep) of formaldehyde is -1.01 V (vs. Ag/AgCl). Formaldehyde in the range 1-1000 micrograms l-1 can be determined. The detection limit for formaldehyde is 0.3 microgram l-1 and the relative standard deviation for the determination of 100 micrograms l-1 formaldehyde was 2.26%. The method was applied to the determination of formaldehyde in environmental samples with satisfactory results.     

Determination of formaldehyde in beverages using microwave-assisted derivatization and ionic liquid-based dispersive liquid-liquid microextraction followed by high-performance liquid chromatography

A simple method based on simultaneous microwave-assisted derivatization and ionic liquid-based dispersive liquid-liquid microextraction (IL-based DLLME) is proposed for the derivatization, extraction and preconcentration of formaldehyde in beverage samples prior to the determination by high-performance liquid chromatography (HPLC). Formaldehyde was in situ derivatized with 2,4-dinitrophenylhydrazine (DNPH) and simultaneously extracted and preconcentrated by using microwave-assisted derivatization and IL-based DLLME in a single step. Several experimental parameters, including type and volume of extraction solvent, type and volume of disperser, microwave power and irradiation time, volume of DNPH, pH of sample solution, and ionic strength were evaluated. When the microwave power was 120 W, formaldehyde could be derivatized and extracted simultaneously only within 90 s. Under optimal experimental conditions, good linearity was observed in the range of 0.5-50 ng/mL with the correlation coefficient of 0.9965, and the limit of detection was 0.12 ng/mL. The proposed method was applied to the analysis of different beverage samples, and the recoveries of formaldehyde obtained were in the range of 84.9-95.1% with the relative standard deviations lower than 8.4%. The results showed that the proposed method was a rapid, convenient and feasible method for the determination of formaldehyde in beverage samples.     

Determination of nickel in water by chemiluminescence

The acetone chemiluminescence determination of nickel in water was investigated. Optimization data for the determination of Ni2+ and interference data for over 20 species are provided. The limit of detection for Ni2+ by this method is 2.5 ng ml-1, and the linear dynamic range is from 10 ng ml-1 to 1 microgram ml-1. The application of the method to the determination of Ni2+ in river and waste waters is discussed.     

Determination of nucleic acids with crystal violet by a resonance light-scattering technique

For the first time, Crystal Violet (CV) was used to determine nucleic acid concentrations using the resonance light-scattering (RLS) technique. Based on the enhancement of the RLS of CV by nucleic acids, a new quantitative determination method for nucleic acids in aqueous solutions has been developed. At pH 5.03 and ionic strength 0.005 mol kg-1, the interaction of CV with nucleic acids results in three characteristic RLS peaks at 344.0, 483.0 and 666.0 nm. With 4.0 x 10(-5) mol l-1 of CV, linear relationships were found between the enhanced intensity of RLS at 666.0 nm and the concentration of nucleic acids in the range 0-2.5 micrograms ml-1 for herring sperm DNA, 0-4.0 micrograms ml-1 for calf thymus DNA and 0-4.5 micrograms ml-1 for yeast RNA. The limits of determination were 13.8 ng ml-1 for herring sperm DNA, 36.8 ng ml-1 for calf thymus DNA and 69.0 ng ml-1 for yeast RNA. The assay is convenient, rapid, inexpensive and simple.     

A new fluorimetric method for the determination of formaldehyde in air based on the liquid droplet sampling technique

A new, simple, sensitive, selective and in-field fluorimetric method for the determination of formaldehyde is proposed. The reaction of formaldehyde with hydralazine in acidic medium, heating on a boiling water-bath for 25 min, produces s-triazolo[3,4-a]phthalazine (Tri-P). The fluorescence intensity of the product formed (Tri-P) was determined at lambda em = 389 nm with lambda ex = 236 nm. The fluorescence intensity is linear over a formaldehyde concentration range of 1.2-33.0 micrograms l-1. The proposed method was applied successfully to the determination of formaldehyde sampled from the atmosphere using the liquid droplet technique. Formaldehyde vapour in a wind tunnel was produced by a mean of permeater. A linear curve was obtained between the concentration in the wind tunnel and that in the droplet. The detection limit for formaldehyde was 2.0 micrograms l-1 with RSDs varying from 3 to 12% in ambient air, using a droplet correction solution (boric acid and hydralazine). The effect of interfering substances on the determination shows that most cations and anions did not interfere. The results obtained were satisfactory compared with a reference method.     

Determination of trace amounts of formaldehyde in acetone

A method to quantify sub-ppm levels of formaldehyde in acetone has been developed and it is reported here. In this method, the different reactivities and stabilities of sulfite with formaldehyde and acetone are used to separate the two carbonyl compounds. Sulfite reacts with formaldehyde to form hydroxymethanesulfonate (HMS), the non-volatile and stable nature of which allows its separation from bulk acetone solvent. The resulting HMS is then converted back to formaldehyde under basic conditions, and formaldehyde is derivatized with 2,4-dinitrophenylhydrazine (DNPH) and quantified in its DNP hydrazone form using high-performance liquid chromatography-UV detection. The method detection limit at the 99% confidence level was 0.051 mg L⁻¹. A batch of samples can be processed within 4 h. The method has been applied to quantify the amount of formaldehyde in an analytical-grade acetone and in a commercial nail polish remover and the level of formaldehyde was found to be 0.175 and 0.184 mg L⁻¹, respectively.     

Spectrophotometric and spectrofluorimetric methods for the determination of tranexamic acid in pharmaceutical formulation

Two simple and sensitive spectrophotometric and fluorimetric methods for the determination of tranexamic acid in tablets are developed. The methods are based on condensation the primary amino group of tranexamic acid with acetyl acetone and formaldehyde producing a yellow coloured product, which is measured spectrophotometrically at 335 nm or fluorimetrically at 480 nm the colour was stable for at least 1 h. Beer's law was valid within a concentration rang of 0.05-2.0 microg ml-1 spectrophotometrically and 0.05-0.25 microg ml-1 fluorimetrically. All the variables were studied to optimize the reaction conditions. No interference was observed in the presence of common pharmaceutical excipints. The validity of both methods was tested by analyzing tranexamic acid in its pharmaceutical preparations. Good recoveries were obtained and the results were comparable with those obtained by standard method.     

Determination of formaldehyde by flow injection analysis with spectrophotometric detection exploiting brilliant green-sulphite reaction

A method for the determination of formaldehyde by flow injection analysis with spectrophotometric detection is proposed, based on retarding the reaction between brilliant green and sulphite by the addition of formaldehyde; this was investigated for formaldehyde quantification in extracts from wood-based panels. For the first time, a heating step was explored, providing a sample throughput of 50 analyses per hour, with a limit of detection of 0.02 mg L^?1 and linearity of 0.20–3.0 mg L^?1, which was adequate for the expected range of formaldehyde concentration in the extracts. The mean recovery observed for actual samples was in the range of 92–106 %, with a maximum relative standard deviation of 6.0 %. The paired t-test revealed no significant difference between this method and the official Nash method, demonstrating an appropriate accuracy and precision; the method is proposed as a simple, fast and inexpensive alternative for the routine determination of formaldehyde in an aqueous medium.