Fluorimetric Determination of p -Hydroxybenzoic Acid in Beer as α -Cyclodextrin Inclusion Complex

Abstract

The inclusion complex of p-hydroxyenzoic acid and α- and β-cyclodextrin has been studied by fluorescence spectroscopy. To describe quantitatively complex formation between α-cyclodextrin (α-CD) and p-hydroxybenzoic acid, an association constant of 967 ± 14 M^?1 at 21°C was obtained. The inclusion complex has been used to determine p-hydroxybenzoic acid in the range 0.15–1.00 mg L^?1 (RSD 4.5%, n = 8). Application of the method to determination of p-hydroxybenzoic acid in beer samples gave an endogenous content of 1.25 mg L^?1.     

β-Cyclodextrin Enhanced Fluorimetric Method for Determination of Amoxicillin in Dosage

A simple sensitive spectrofluorimetric method was developed for the determination of amoxicillin. Amoxicillin in the presence of formaldehyde produces a fluorescent pyrazine derivative, whose fluorescence intensity can be enhanced by forming an inclusion complex with β-cyclodextrin. Optimum conditions for the determination of amoxicillin were also investigated. Fluorimetric detection was carried out at λex=365 nm and λem=445 nm. The linear range of this method for the determination of amoxicillin is 0.1―10 ...     

Enzymatic Determination of Urinary Total 17β-Hydroxysteroids

Abstract

An enzymatic determination of urinary total 17β-hydroxysteroids is described. The principle of the method is as follows: after hydrolysis with β-glucuronidase and solvolysis, the ethyl acetate layer, which is washed with alkaline solution and water, is transferred to two test tubes, then each of them is evaporated. To one test tube is added 3β,17β-hydroxysteroid dehydrogenase (EC 1.1.1.51, from P. testosteroni), NAD⁺, 2-ρ-iodophenyl-3-ρ-nitrophenyl-5-phenyltetrazolium chloride (INT), and diaphorase (EC 1.6.99.2, from C. kluyveri) for determination of total 3β,17β-hydroxysteroids. To another test tube is added 3β-hydroxysteroid oxidase (EC 1.1.3.6, from B. sterolicum) for determination of total 3β-hydroxysteroids. The value of 17β-hydroxysteroids is calculated by subtracting the value for 3β-hydroxysteroids from the value for the 3β,17β-hydroxysteroids.     

Oligomeric Derivatives of 3α,7β-D Ihydroxy-5β-Cholan-24-Oic Acid (Ursodeoxycholic Acid)

The synthesis and pharmacological evaluation of Oligomeric and polymeric derivatives of drugs is receiving increasing attention by several groups ^1-9. Usually, in these derivatives, the drug moieties are linked to a proper oligomeric or polymeric matrix by means of covalent bonds of limited stability to biological environments. This may ensure a gradual release of the active principle after introduction into the body Fluids. Poly(oxyethyleneglycol)s, as matrices, appear to be particularly promising on this respect⁷.     

Voltammmetric Determination of Uric Acid in the Presence of Ascorbates Using Overoxidized Polypyrrol

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Chemiluminescence Determination of Benzoic Acid Using A Solid-Phase Verdigris Reactor

Benzoicacidisacommonadditiveusedwidelyasfoodpreservativeandplasticizer.Itcouldpromoteseverereactiontoallergicpopulationevenatlowconcentrationlevel1.Routinemethodsfortheassayofbenzoicacidincludeschromatographic2-6,spectrophotometry7,8,capillaryelectrophoresis9-13andelectrochemicaltitration14.Stokes15etal.monitoredairbornebenzoicacidbasedonsurface-enhancedRamanscatteringtechniques.Thereisalsoreportonamicrobialsensorusingpseudomonasforbenzoicacidandtheirderivativesinaqua16.Interestofusinglumines…     

Spectrofluorimetric Determination of Kinetic Parameters of Bile Acids With 3α-Hydroxysteroid Dehydrogenase from Mutant Pseudomonas Testosteroni

Abstract

The spectrofluorimetric determination of kinetic parameters (K_m, V and k_obs) of conjugated bile acids with 3α-hydroxysteroid dehydrogenase from mutant Ps. Testosteroni is described. Under optimal pH conditions and pseudo- first order kinetics([β-NAD⁺)20 K_mNAD+) the kinetic parameters of bile acids in different buffers are determined. The bile acids exhibit larger kinetic differences in glycine and Tris buffer compared to those measured in pvrophosphate buffer. From these data it is concluded that under certain conditions the differential kinetic determination of one bile acid in the presence of others is possible without prior separation.     

Enzymatic Determination of Urinary Total 7α-Hydroxy Bile Acids

Abstract

An enzymatic determination of urinary 7^α-hydroxy bile acids is described. The principle of the method is as follows: after hydrolysis with β-glucuronidase and solvolysis, the ethyl acetate extract is washed with alkalin solution and water, then the alkali and water washes of the ethyl acetate extract are combined and the solution is acidified to pH 1 and sodium chloride added. Shake solution with ethyl acetate to re-extract the acidic fraction and the ethyl acetate layer is evaporated. Add enzyme color solution of 7_α-hydroxysteroid dehydrogenase (7_α-HSD, from E. coli) to a tube of extract residue and then after incubation, measure the absorbance of the solution.

Excretion values of urinary total 7_α-hydroxy bile acids was measured with patients of acute hepatitis and normal subjects and excretion pattern of 7_α-hydroxy bile acids by the use of chromatographic fractionation was also shown.     

Near-Infrared Fluorimetric Determination of Copper(Ⅱ) Ions Using CdHgTe Nanorods as Probe

Stable water‐soluble CdHgTe nanorods with an emission wavelength at 722 nm, obtained by doping Hg²⁺ into CdTe nanorods, has been used as a near‐infrared region (NIR) probe to investigate their interaction with copper(II) ions. A new fluorimetric method for the determination of copper(II) ions has been developed based on the quenching effect of copper(II) ions on the emission of CdHgTe nanorods. The mechanism studies show that an effective electron transfer from nanorods to the copper(II) ions occurred based on the coordination reaction between copper(II) ions and the carboxyl groups on the nanorods surface, which could be responsible for the emission quenching of CdHgTe nanorods. Under optimum conditions, the linear range of the calibration curve for the determination of Cu²⁺ is from 8.0×10^?9 to 1.0×10^?6 mol/L and the detection limit is 2.0×10^?9 mol/L. Owing to low background interference of NIR measurement, the proposed method displays relative high sensitivity and selectivity. Especially, some physiologically important cations almost do not interfere with the determination of Cu²⁺. The proposed method was also applied to the determination of trace Cu²⁺ in real aqueous samples with satisfactory results.     

Fabrication of CeO2 Nanoparticle Modified Glassy Carbon Electrode for Ultrasensitive Determination of Trace Amounts of Uric Acid in Urine

The preparation of a glassy carbon electrode modified by CeO2 nanoparticles was described, which was characterized by cyclic voltammetry and electrochemical impedance spectroscopy. In pH 6.0 buffer, the CeO2 nanoparticle modified electrode （CeO2 NP/GC） gave an excellent electrocatalytic activity for the oxidation of uric acid （UA）. The catalytic current of UA versus its concentration had a good linear relation in the range of 2.0 × 10^-7-5.0 × 10^- 4 mol/L, with the correlation coefficient of 0.9986 and detection limit of 1.0 ×10^-7 mol/L. The modified electrode can be used for the determination of UA in urine, which can tolerate the interference of ascorbic acid up to 1000-fold. The method was simple, quick and sensitive.     

Simultaneous Capillary Gas Chromatographic Determination of Cyproterone Acetate and 15β-Hydroxycyproterone Acetate in Urine

Abstract

The simultaneous capillary GC determination of underivatized antiandrogen cyproterone acetate (CPA) and its active metabolite 15β-hydroxycyproterone acetate (OH-CPA) in spiked urine was performed on a flexible VCOT quartz capillary column, coated with a non-polar CP-Sil 5 CB liquid phase. A split/splitless injector and a flame-ionization detector were used. Equilin was used as an internal standard, and resolution of all the compounds was achieved in 6 minutes. Limit of detection was 0.04 μg/μl of injected amount for both CPA and OH-CPA, the recoveries were between 91.35% and 105.56%, and the relative standard deviation varied from 3.35% to 7.38%. The method is applicable in analysis of these steroids in biological fluids.     

LC–MS/MS Determination of Catecholamines in Urine Using FMOC-Cl Derivatization on Solid-Phase Extraction Cartridge

A method for the determination of catecholamine derivatives in human urine is proposed that includes the derivatization of target compounds on a solid-phase extraction cartridge and determination of the analytes by a UHPLC method with tandem mass-spectrometric detection. 9-Fluorenyl-methoxycarbonyl chloride was used as the derivatization agent. The limits of detection for the analytes were 2.5 ng mL^?1 for 9-fluorenyl-methoxycarbonyl-adrenaline, 5 ng mL^?1 for 9-fluorenyl-methoxycarbonyl-octopamine, and 25 ng mL^?1 for 9-fluorenyl-methoxycarbonyl-dopamine. The proposed procedure was tested on real samples obtained from volunteers.     

Synthesis of A High Molecular Weight Polymeric Die Rivative of 3α,7β-Dihydroxy-53-Cholan-24-Oic Acid (Ursodeoxycholic Acid)

In another paper¹ we have reported the synthesis of cligomeric poly(oxyethyleneglyccl) derivatives of the title compound. One of these derivatives was orally administered to human volunteers, and proved to be able to give much higher and more sustained blood levels of Urscdecxycholic acid (UDCA) than the free acid, if given in equivalent doses. This prompted us to study also high molecular weight polymeric derivatives of UDCA.     

Electrochemical Determination of Propranolol,Acetaminophen and Folic Acid in Urine,and Human Plasma Using Cu2O–CuO/rGO/CPE

Russian Journal of Electrochemistry - A Cu2O–CuO/rGO/CPE was used for simultaneous measurement of propranolol (PRO), Acetaminophen (AC) and folic acid (FA) using differential pulse...     

Highly Sensitive Determination of Traces of Co(II) in Pharmaceutical and Urine Samples Using Kinetic–Spectrophotometric Method

Abstract

A high sensitive, accurate and simple kinetic method has been developed for determination of trace of Co(II) ions, based on its strongly catalytic effect in the reaction oxidation of disodium-6-hydroxy-5-[(4-sulfophenyl)azo]-2-naphtalenesulfonic acid (artificial color, Sunset Yellow FCF, E110 in text selected as SY) by hydrogen peroxide in borate buffer at pH of 9.5, by monitoring the rate of disappearance of SY. Reaction rate was monitored spectrophotometrically, at λ_max of the SY at 478.4 nm. The optimum operating conditions regarding reagents concentration and temperature were established. The tangent method was adopted for constructing the calibration curve, which was found to be linear over the concentration range 1.18–17.67 ng ml^?1 and 17.67–58.90 ng ml^?1 of Co(II). The limit of detection (3σ) is 0.15 ng ml^?1, and limit of quantification (10σ) is 0.5 ng ml^?1. The effects of the other ions on the reaction rate were determined for an assessment of the selectivity of the method. The developed kinetic procedure was successfully applied for the determination of Co(II) in pharmaceutical and urine samples. The unique features of this procedure are that the determination can be performed at room temperature, and the analysis time is short. The newly developed method is high sensitive, simple, inexpensive and efficient for use in the analysis of a large number of samples.     

Determination of γ-Aminobutyric Acid in the Mouse Hypothalamus and Hippocampus Using Liquid Chromatography/Electrochemistry

Abstract

A method is described for the rapid detection and measurement of γ-aminobutyric acid (GABA) in crude extracts of mouse brain. This study includes optimisation of the pre-column derivatization of GABA by o-phthalaldehyde in the presence of ethylmercaptan as well as of the chromatographic and electrochemical conditions. The GABA levels have been measured in the hypothalamus and hippocampus of control mice and mice treated with three compounds known for their activity on brain GABA levels.     

Simultaneous Determination of 6β-Hydroxycortisol and 6β-Hydroxycortisone in Human Urine by LC with UV Absorbance Detection

A liquid chromatographic method for the simultaneous determination of 6β-hydroxycortisol and 6β-hydroxycortisone using dexamethasone as internal standard in human urine is described. Separation was achieved on a reversed-phase C18 column by a gradient elution of acetonitrile and water containing 0.1% formic acid. 6β-Hydroxycortisol and 6β-hydroxycortisone were monitored by UV absorption at 244 nm. The lower limits of quantitation were 5 ng mL^?1 for both analytes. The intra-day and inter-day relative standard deviations were less than 7.4%. Accuracy determined at three concentrations ranged between 92.16 and 109.77%. The sensitivity, specificity and accuracy of this method were demonstrated to be satisfactory for measuring both metabolites in human urine.     

Determination of Phytate in Urine by High-Performance Liquid Chromatography–Mass Spectrometry

An indirect method is described for determination of phytate in human urine. The method is based on hydrolysis of the phytate and determination of myo-inositol, one of the hydrolysis products. Chromatographic separations were performed on an Aminex HPX-87C column with Milli-Q water as mobile phase; 5 mM ammonium acetate was added post-column. The detector counted positive ions by monitoring m/z=198, which corresponds to the adduct of myo-inositol with the ammonium cation. The relative standard deviations obtained for standards containing 0.5, 1, and 1.5 mg L^–1 phytate were 4.1, 3.0, and 2.7% respectively (n=5). The limit of detection was 60 g L^–1. Different urine samples were analyzed both by this method and by an alternative analytical method based on GC–MS. The results from both methods were comparable.     

High Pressure Liquid Chromatography Assay for Determination of 18-β-Glycyrrhetinic Acid in Plasma

Abstract

This report presents a useful high pressure chromatography assay for determination of the proposed chemopreventive agent 18-β-glycerrhetinic acid (GA) in murine and human plasma. Drug was released from plasma proteins through precipitation with a mixture of sodium bisulfate and sodium chloride after which it was extracted with acetonitrile. Standard calibration curves of GA covered the concentration range of 2.5 to 120 μg/ml. The lower limit of detection was 0.5 μg/ml. No endogenous plasma constituents from plasma were found to interfere with the determination of GA. Recover of GA from plasma was greater than 95% over a concentration range of 20 to 100 μg/ml. Linearity of the assay was excellent; within-run precision showed a C.V. of 4.2% at 25 μg/ml, 5.6% at 20 μg/ml and 3.4% at 120 μg/ml. Between-run assay precision and accuracy was also considered to be excellent. The specificity, sensitivity and reproducibility of the procedure are adequate for proposed clinical pharmacology studies of this agent.