Enzymic method for the spectrophotometric determination of choline in liquor.

A sensitive spectrophotometric method for the determination of choline in liquor is described. The method involves the conversion of choline into formaldehyde by sequential enzymic reactions (choline oxidase and catalase), followed by the formation of a chromophore with 4-aminopent-3-en-2-one. The calibration graph was linear in the range 0.4-15 micrograms cm-3 of choline. The relative standard deviation at 5 micrograms cm-3 of choline was 1.3%. There was no interference from most of the common ingredients of liquor. More than 95% of choline added at two levels was recovered from real samples. The method is simple, and the detection limit was 2 micrograms g-1 when 5 g of sample were assayed.     

A novel spectrophotometric method for batch and flow injection determination of sulfite in beverages

A novel spectrophotometric assay method for batch and flow injection determination of sulfite in beverages is described. The method involves a reaction with diaquacobyrinic acid heptamethyl ester (diaquacobester, DACbs) in acetate buffer of pH 3 to form a highly stable sulfite cobester complex (SO₃Cbs). In the absence of sulfite, the reagent displays three absorption maxima at 349, 409 and 525 nm. Addition of sulfite is associated with the development of a new absorption band at 313 nm, an increase in the intensity of the band at 425 nm and a decrease in the absorbance of the bands at 349 and 525 nm. Variations of the absorptions at 313, 349, 425 and 525 nm are linearly proportional to sulfite concentrations over the range of 0.05–25 μg ml⁻¹with a detection limit of 0.01–0.2 μg ml⁻¹. Negligible interferences are caused by most common ions. Validation of the method according to the quality assurance standards shows suitability for quality control assessment of sulfite in complex matrices without prior treatment. The method has the advantages of high selectivity, good sensitivity, fast reaction, high stability of the reagent and reaction product and absorbance measurements at four different wavelengths in the same run. The method is successfully applied to determine the sulfite contents of some beverages. The results compare fairly well with data obtained using the standard method.     

Flow-through spectrophotometric sensor for the determination of aspartame in low-calorie and dietary products.

A very simple flow-through sensor is presented for the determination of the intense sweetener aspartame in low-calorie and dietary products. The sensor is implemented in a monochannel flow-injection system with UV spectrophotometric detection using a Sephadex CM-C25 cationic exchanger packed 20 mm high in a flow cell. This method is based on the transient retention of a cationic species of the sweetener on the solid phase when a pH 5.0 acetic acid sodium acetate buffer (0.01 M) is used as a carrier (2.6 mL(-1) min). The carrier itself elutes the analyte from the solid support, regenerating a sensing zone. Aspartame was determined by measuring its intrinsic absorbance at 219 nm at its residence time without any derivatization. Calibration graphs were linear over the range of 5.0 - 600.0 microg mL(-1) with an RSD of 0.55% (peak height). This sweetener was determined in several samples by measuring the height or peak area, obtaining recoveries ranging between 95 - 101% and 97.5 - 101%, respectively. The procedure was validated for its use in the determination of aspartame in low-calorie and dietary products, giving reproducible and accurate results.     

Amplification method for the spectrophotometric determination of phosphorus

An amplification method with ion-exchange pre-separation for the spectrophotometric phosphorus determination in various alloys is described. Phosphorus is converted into molybdophosphoric acid, separated by selective extraction and back-extracted into the aqueous phase. The molybdenum is liberated by alkaline decomposition of the heteropoly acid. The spectrophotometric measurement is based on the reaction of molybdenum(VI) with 2,2-biquinoxalyl. High molar absorptivity of 1,1-dihydro-2,2-biquinoxalylene (=3.3 · 10⁴ L mol^–1 cm^–1) and the twelve-fold amplification guarantee high precision and makes the determination of phosphorus in the 1–6 g level possible.     

A spectrophotometric method for the determination of nickel

A photometric method for the determination of nickel using versene is described. Up to 20 mg of nickel can be determined with a maximum deviation of ± 0.10 mg. The effect of interfering elements, concentrations, accuracy and limitations of the method are discussed.     

A spectrophotometric method for the determination of nitrite

Nitrite reacts with dichromate quantitatively under suitable conditions of temperature and acid concentration. A linear relationship was found to exist between nitrite concentration and the absorbance at 580 nm of the chromium (III) species produced. This was used to determine the nitrite. The influence of a number of ions on the determination of nitrite was investigated; up to 100-fold excess nitrate has no influence on the determination of nitrite.     

甲酚红褪色分光光度法测定吡罗昔康

用褪色分光光度法(测定药物制剂和生物样品中吡罗昔康含量。)在pH8.75的tris-HCl缓冲溶液中,甲酚红与吡罗昔康反应形成离子缔合物,使甲酚红溶液褪色,最大褪色波长位于570nm,吡罗昔康浓度在0.06628～11.60μg/mL范围内遵循比尔定律,回归方程为ΔA=0.1404c+0.0067,相关系数为r=0.9996,表观摩尔吸光系数为4.703×104L·mol-1.cm-1。据此建立了方法,样品测定平均回收率为97.51%～101.4%。     

甲酚红褪色分光光度法测定芬布芬的研究及其应用

在pH9.00的tris-HCl缓冲溶液中,甲酚红与芬布芬反应形成离子缔合物,使甲酚红溶液褪色.实验结果表明:最大褪色波长位于569.0nm,芬布芬浓度在0.05086～10.17μg/mL范围内遵循比尔定律,回归方程为ΔA=0.1702c+0.0107(c=μg/mL),相关系数为r=0.9996,表观摩尔吸光系数为4.537×104 L·mol-1·cm-1.据此建立了测定药物制剂和生物样品中芬布芬含量的褪色分光光度法,样品测定平均回收率为97.97%～101.6%.     

Versatile spectrophotometric method for the determination of silicon

A versatile spectrophotometric method is described for the determination of microgram levels of silicon, as molybdenum blue. It combines the desirable features of existing spectrophotometric methods with three pretreatment procedures, namely (a) the removal of cations with a cation-exchange resin in the H(+)-form, (b) the conversion of all silicon species into the reactive monomer with an alkaline treatment, and (c) the decomposition of silicon fluoride with boric acid in the presence of cation-exchange resin. These pretreatments coupled with the colour development provide five procedures which are applicable to a wide variety of samples including natural and industrial waters and solutions of various nuclear reactor fuels and components. Provisions are included for the selective determination of total silicon.     

A spectrophotometric method for uranium determination

A very sensitive extraction spectrophotometric method for the analysis of uranium based on the extraction of a uranium—benzoate—crystal violet complex by a mixture of xylene and benzene is described. The absorbance maximum is at 606 nm and molar absorptivity is 4.28·10⁴ l·mol⁻¹·cm⁻¹. The interference due to a number of anions and cations studied without any pre-extraction was found to be within permissible limits. The method has been used for determining uranium in a synthetic solution, i.e., uranium in the presence of various other ions. The interference due to some cations was eliminated by the use of a masking agent (boric acid).     

New spectrophotometric method for determination of cephazolin

A simple, selective and accurate spectrophotometric method has been developed for the determination of the cephalosporin-type antibiotic cephazolin. The method is based on the fast preliminary acid hydrolysis of cephazolin and the spectrophotometric determination of one of its degradation products-2-mercapto-5-methylthiadiazole.     

A sensitive method for the determination of nitroamines in alcoholic beverages

Summary Nitrosamines in alcoholic beverages and malted barley were analysed by adsorption from the gas phase onto a porous polymer trap of Chromosorb 104 and subsequent desorption of the trapped compounds directly to a gas chromatograph fitted with glass capillary column and alkali-FID. The detection limit for NDMA was 0.05 g/l in beer samples and 0.3 g/kg in malted barley.Presented at the 14th International Symposium on Chromatography London, September, 1982     

Extractive spectrophotometric method for the determination of niobium in steels

A strongly coloured complex of niobium with PAR is formed in oxalate solutions and at pH 7.4 can be extracted into nitrobenzene as an ion-association complex with xylometazolonium ion (XMH), with a molar absorptivity of 46300 1 mol^–1 cm^–1 at 545 nm. In contrast to cationic extractants such as tetraphenylphosphonium or tetraphenylarsonium chloride, XMH is an effective extractant over a wide concentration range without any difficulties in either the separation of the phases or the absorbance of the reagent blank. Job's method of continuous variations revealed that the composition of the extracting species as 1 1 1 1 for niobium oxalate PAR XMH. Based on this extraction, a highly sensitive and selective spectrophotometric method for the determination of niobium in various steels, after prior separation of iron, is described. 4-(2-Pyridylazo)resorcinol (PAR) reacts with the niobium tartrate complex in nearly neutral medium to form a red, water-soluble 1 1 anionic complex [1]. PAR is an unselective reagent and one way of improving selectivity is by ternary and ion-association complex formation. The extraction of some highly coloured metal-PAR complexes with tetraphenylarsonium or tetraphenylphosphonium ion has been described [2, 3]. The PAR complex of niobium, which is formed in oxalate solutions has been shown to be extractable by chloroform using tetraphenylarsonium and phosphonium salts [4, 5]. However, in many of these extraction spectrophotometric procedures difficulties arise due to the delay in the separation of the two phases and significant absorbance of the reagent blank solution, particularly when concentrated solutions of reagents are used.The extraction of anionic complexes of Pd, V, and Cr with xylometazolonium (XMH) cation has been reported elsewhere [6–9]. In the present study we have tried to extract Nb(V) and it is observed that 1 1 oxalatoniobium-PAR complex can be extracted with XMH. A method is proposed for the determination of niobium in standard steels.     

A simple spectrophotometric method for the determination of minoxidil

A simple and sensitive method for the determination of minoxidil using 3-methyl-2-benzothiazolinone hydrazone (MBTH) and Fe(III) as the coloring agent is described. The method is sensitive to permit the determination of 0.5–4.5 μg ml⁻¹ of minoxidil at 500 nm. The accuracy and precision of the method were checked by high-performance liquid chromatography.     

A spectrophotometric method for the determination of nitric oxide

In dimethylsulfoxide, nitric oxide reduces copper(II) to copper(I) in the presence of p-chloroaniline. The resulting copper(I) is determined spectrophotometrically with 2,2′-biquinoline. The reactions are reproducible and the absorbance is proportional to the concentration of nitric oxide over the range 1.8–108 ppm (mg dm^?3. Most other atmospheric contaminants are without effect.     

A solid-phase spectrophotometric method for the determination of sulphathiazole

A spectrophotometric method for the determination of sulphathiazole (ST) has been developed, based on solid-phase spectrophotometry. The influence of experimental variables on fixation on Sephadex SP C-25 is discussed. The applicable concentration range is 0.10-10.00 mg/l., with a relative standard deviation of 0.62% and a detection limit of 0.02 mg/l. The accuracy and precision of the method are reported. The proposed method has been satisfactorily applied to the determination of sulphathiazole in pharmaceuticals.     

A new spectrophotometric method for the determination of nadolol

A new spectrophotometric method has been developed for the assay of nadolol in pure form and in tablets. The assay procedure is based on a derivatization methodology employing 4-carboxyl-2,6-dinitrobenzene diazonium ion (CDNBD) as a diazo coupling reagent. The azo dye formed between nadolol and CDNBD absorbed visible light at the wavelength maximum of 416 nm (λ_max) demonstrating a bathochromic shift from the absorption maximum of nadolol. Optimization studies established an optimal reaction time of 10 min at 60 °C. The assays were linear over 1.25–10 μg ml^?1 of nadolol, and the reaction occurred by a 3:1 reagent/drug stoichiometric ratio. The method is found to be selective and has a lower detection limit of 0.29 μg ml^?1. Recovery studies over three days gave mean recovery of 101.4% (RSD 3.0%). This new method has been successfully applied in the determination of nadolol and nadolol/bendroflumethiazide tablets with accuracy and precision similar to the official (USP) HPLC procedure (p > 0.05). The new procedure has the advantages of high sensitivity, lower limit of detection and could find application as an in-process quality control method for nadolol.     

New spectrophotometric method for the determination of phenolic hormones

A new simple, selective and accurate spectrophotometric method is described for the determination of mono- and dihydric phenolic hormones (oestrogens and catecholamines) by nitration at 50 degrees and 100 degrees , respectively, for 10 min, followed by treatment with alkali. Coloured products with absorption maxima at 430, 385, 430, 380 and 380 nm, linearly proportional to the concentration of oestrone, oestradiol, ethinyloestradiol, adrenaline and noradrenaline, respectively, are obtained. Information is presented on the effect of nitration time, temperature, solvents, and alkali concentration. The method is satisfactorily applied to the determination of these hormones in the range 10-50mug ml in the final solution, of volume 10ml. The relative standard deviation is +/- 0.5% and no interferences are caused by non-phenolic hormones.     

Extraction-visible spectrophotometric method for the determination of tetraphenylphosphonium salts

Das empfindliche und relativ einfache Verfahren beruht auf der Extraktion des Tetraphenylphosphonium-Kations mit dem Vanadium(V)-4-(2-pyridylazo)-resorcin-Komplex und Absorptionsmessung der gefärbten organischen Phase bei 560 nm (molarer Extinktionskoeffizient 3,9 · 10⁴ l · mol^?1 · cm^?1). Das Lambert-Beersche Gesetz wird im Bereich von 1 · 10^?6 ?5 · 10^?5 M Tetraphenylphosphonium im Extrakt befolgt. Die relative Standardabweichung beträgt ±2% im Bereich von 10^?5 M und 5–10% im Bereich von 10^?6 M. Die Methode ist empfindlicher und weniger störanfällig als die direkte UV-Methode.