Up-to-date studies regarding the determination of melatonin by chromatographic methods.

Melatonin is an indolic compound that has been reported in the literature to exist in human-based samples, vertebrates, vegetables, fruits, and pharmaceutical products. Melatonin is considered a dietary supplement and can regulate circadian rhythms, although it has not been classified as a drug by the US Food and Drug Administration. Several analytical methods have been used for its detection. This study aimed to summarize the recent outcomes of the chromatographic methods such as electrophoretic methods, gas chromatography, and liquid chromatography, which have been used for the determination of melatonin in the last three decades, with the focus on gas chromatography and high-performance liquid chromatography methods.

Rapid, sensitive, and selective copper (II) determination using sensitive chromogenic azo dye based on sulfonamide.

A simple methods have been developed for determination of Cu(II) ions in aqueous solutions. The spectrophotometric method relied mainly on the reaction between Cu(II) ions and the azo dye ligand named N-diaminomethylene-4-(2,4-dihydroxy-phenylazo)-benzenesulfonamide (H2L) at pH 10.0. The influence of parameters such as concentration, pH and reaction time were inspected. A linear relationship (R2 = 0.9992) between absorbance and the concentration of Cu(II) was obtained at themaximum absorptionpeak of 474 nm within 1.6-9.6 × 10-6 mol L-1 concentration range. The limit of detection for Cu(II) ion and limit of quantitation were 1.1 × 10-7 mol L-1 and 3.7 × 10-7 mol L-1, respectively.The potentiometric method is based on a novel poly(vinyl chloride) membrane, containing the synthesized azo dye as an ionophore, was used to developed a Cu(II)- selective sensor. This newly developed sensor revealed a Nernstian response over Cu2+ ion in a concentration range 1.0 × 10-6-1.0 × 10-2 mol L-1 with cationic slopes of 29.5 ± 0.2 mV decade-1 and detection limits of 3.0 × 10-6 mol L-1 copper(II) for o-nitrophenyl-octyl ether (o-NPOE) based membrane sensor. The electrode showed good discrimination toward Cu2+ ions with respect to most common cations. The advantages of the proposed methods are their simplicity, selectivity, and high sensitivity. In addition, the sensor has been used as indicator electrode in the potentiometric titration of Cu2+ ion against EDTA. The structure and geometry of the complex formed between Cu(II) and H2L ligand was identified via isolation of the solid complex; Co(II) an Ni(II) complexes were synthesized as well. The geometrical structure around the metal centers were proved to be square planar for Cu(II) complex and tetrahedral for Co(II) an Ni(II) complexes.

Study on solid phase extraction and spectrophotometric determination of vanadium with 2,3-dichloro-6-(2,7-dihydroxy-1-naphthylazo)quinoxaline.

A sensitive, selective and rapid method has been developed for the determination micrograms per liter level of vanadium ion based on the rapid reaction of vanadium(V) with 2,3-dichloro-6-(2,7-dihydroxy-1-naphthylazo)quinoxaline (DCDHNAQ) and the solid phase extraction of the colored complex with C18 cartridge. The DCDHNAQ reacts with V(V) in the presence of citric acid-sodium hydroxide buffer solution (pH 3.3) and benzyldimethyl tetradecylammonium chloride (zephiramine) medium to form a violet complex of a molar ratio 1:2 [V(V) to DCDHNAQ]. This complex was enriched by solid phase extraction with C18 cartridge and the enrichment factor of 100 was obtained by elution of the complex from the cartridge with acetonitrile. The molar absorptivity and Sandell sensitivity of the complex are 2.45x10(5) L mol(-1) cm(-1) and 0.0208 ng cm(-2) at 573 nm in the measured solution. Beer's law is obeyed in the range of 0.01-0.45 microg mL(-1), whereas Ringbom optimum concentration ranges found to be 0.025-0.425 microg mL(-1). The detection and quantification limits are 3.2 and 9.9 microg L(-1), respectively in the original samples. This method was applied to the determination of vanadium(V) in steel, soil, water and biological samples with good results.

On-line solid phase extraction coupled to capillary LC-ESI-MS for determination of fluoxetine in human blood plasma.

An instrumental setup including on-line solid phased extraction coupled to capillary liquid chromatography-electrospray ionization-mass spectrometry (SPE-capLC-ESI-MS) has been constructed to improve the sensitivity for quantification of fluoxetine hydrochloride in human plasma. Prior to injection, 0.5 mL of plasma spiked with metronidazole (internal standard) was mixed with ammonium formate buffer for effective chloroform liquid-liquid extraction. The method was validated in the range 5-60 ng mL(-1) fluoxetine, yielding a correlation coefficient of 0.999 (r(2)). The within-assay and between-assay precisions were between (8.5 and 11%) and (6.6 and 7.5%), respectively. The method was used to determine the amount of fluoxetine in a healthy male 14 h after an intake of one capsule of the antidepressant and anorectic Flutin, which contains 20mg fluoxetine per each capsule. Fluoxetine was detected, and the concentration was calculated to 9.0 ng mL(-1) plasma. In the preliminary experiments, conventional LC-UV instrumentation was employed. However, it was found that employing a capillary column with an inner diameter of (0.3mm I.D. x 50 mm, Zorbax C(18)) increased the sensitivity by a factor of approximately 100, when injecting the same mass of analyte. Incorporating an easily automated C(18) reversed phase column switching system with SPE (1.0mm I.D. x 5.0mm, 5 microm) made it possible to inject up to 100 microL of solution, and the total analysis time was 5.5 min.