Lorena L. Sombra

Determination of melatonin in wine and plant extracts by capillary electrochromatography with immobilized carboxylic multi-walled carbon nanotubes as stationary phase

The finding of melatonin, the often called “hormone of darkness” in plants opens an interesting perspective associated to the plethora of health benefits related to the moderate consumption of red wine. In this study, the implementation of a new method for the determination of melatonin in complex food matrices by CEC with immobilized carboxylic multi‐walled carbon nanotubes as stationary phase is demonstrated. The results indicated high electrochromatographic resolution, good capillary efficiencies and improved sensitivity respect to those obtained with conventional capillaries. In addition, it was demonstrated highly reproducible results between runs, days and columns. The LOD for melatonin was 0.01 ng/mL. The method was successfully applied to the determination of melatonin in red and white wine, grape skin and plant extracts of Salvia officinalis L.

Spectrophotometric determination of trace aluminium content in parenteral solutions by combined cloud point preconcentration–flow injection analysis

A cloud point preconcentration and flow injection (FI) analysis methodology for aluminium(III) determination has been developed. The analyte in the initial aqueous solution was complexed with Chrome Azurol S (CAS) in the presence of the cationic surfactant benzyldimethyltetradecylammonium chloride (BDTAC). The absorption spectroscopic characteristics of the ternary complex [Al(III)-CAS-BDTAC] were examined in detail. The preconcentration step was carried out by means of the non-ionic surfactant polyethylene glycol p-nonylphenyl ether (PONPE 7.5). The enriched analyte solution was injected into an FI system using an HPLC pump. The chemical variables affecting the analytical performance of the combined methodology were studied and optimised. The developed approach was successfully applied to the determination of trace amounts of aluminium in parenteral solutions without previous treatment. Under the optimum experimental conditions, 99.9% extraction was achieved for a preconcentration factor of 50. The limit of detection was 1.12 x 10(-7) mol(-1). The calibration plot was linear over at least two orders of magnitude of aluminium concentration. The developed coupled methodology, which thoroughly satisfies the typical requirements for pharmaceutical control processes, is appropriate for monitoring the aluminium concentration in parenteral nutrition.

Assessment of trace aluminium content in parenteral solutions by combined cloud point preconcentration—flow injection inductively coupled plasma optical emission spectrometry

A micelle-mediated phase separation without added chelating agents to preconcentrate trace levels of aluminium in parenteral solutions as a prior step to its determination by flow injection inductively coupled plasma optical emission spectrometry has been developed. The enrichment step is based on the cloud point extraction of aluminium with the non-ionic surfactant polyethyleneglycolmono-p-nonylphenylether (PONPE 7.5). The chemical variables affecting the sensitivity of the extractive-spectrometric procedure were studied in detail. After optimization, a preconcentration factor of 200 and a %E higher than 99.9 were achieved. The detection limit (DL) value of aluminium for the preconcentration of 50 ml of parenteral solution was 0.25 microgl(-1). The calibration graph using the preconcentration system for aluminium was linear with a correlation coefficient of 0.9997 at levels near the DLs up to at least 200 microgl(-1). The developed hyphenated assay, which thoroughly satisfies the typical requirements for pharmaceutical control processes, is appropriate to monitor the aluminium concentration in parenteral nutrition.

A combination of single-drop microextraction and open tubular capillary electrochromatography with carbon nanotubes as stationary phase for the determination of low concentration of illicit drugs in horse urine

In this study we developed an interesting alternative to HPLC-mass spectrometry for the quantification of seven important drugs of abuse in racehorses. The procedure proposed in this work is a combination of single-drop microextraction (SDME) and an open tubular capillary electrochromatography (OT-CEC) using multi-wall carbon nanotubes (MWCTs) immobilized into a fused-silica capillary as a stationary phase. The SDME showed to be a powerful tool for extraction/preconcentration of the seven drugs analyzed in the study, showing an enrichment factor between 38- and 102-fold depending on the drug. We have investigated the electrophoretic features of MWCTs immobilized fused-silica capillary by covalent modification of the inner surface of the capillary. The results show a good run-to-run, day-to-day and capillary-to-capillary reproducibility of the method. Compared with the capillary zone electrophoresis (CZE), the coating of the capillary allowed the separation of the analytes with high resolution, with less band-broadening and without distortion of the baseline. The interactions between the analytes and the MWCTs resulted in an increased migration time and probably this was the reason of the front tailing effect. The results showed a good capillary efficiencies and an improved of the electrophoretic separation.

A New Fluorescent Assay for Enalapril Maleate

A new spectrofluorimetric method for the enalapril maleate monitoring was studied. Enalapril maleate was found to be highly photolabile. This drug was evaluated according to photodegradation assay at pH 2.5 and 6. Enalapril maleate was exposed to UVA–UVB radiations. Under these specific conditions was found as degradation product, the diketopiperazine. The modification of the fluorescent properties of enalapril maleate in solution after exposure UV-radiation and the degradation mechanisms were studied. The photodegradation was followed by the developed spectrofluorimetric assay.

Analysis of nordihydroguaiaretic acid in Larrea divaricata Cav. extracts by micellar electrokinetic chromatography.

INTRODUCTION Larrea divaricata Cav. is a common shrub used in folk medicine to treat a variety of diseases. The main product extracted from this bush is nordihydroguaiaretic acid (NDG), which is a potent antioxidant. OBJECTIVE In this paper we propose a novel method for the quantification of NDG in different extracts of Larrea divaricata. The concentration of NDG in two different aqueous extracts (I and D) and an ethanolic extract (Eet) was analysed, in order to evaluate the safe use of the extracts for pharmacological purposes. METHODOLOGY Micellar electrokinetic chromatography (MEKC) was performed under the following conditions: the background electrolyte used consisted of 20  mm phosphate buffer (pH 7.5), 10  mm sodium dodecyl sulphate and 10% acetonitrile. RESULTS The limits of detection and quantitation of NDG were 4.54 × 10(-4) and 10.6 × 10(-4)   mg/mL, respectively. The concentration of this acid in both aqueous extracts was within the safe levels. However, the decoction must be used carefully because the concentration of the acid was almost over the recommended limit. In the case of ethanolic extracts, the amount of NDG was above the safe concentration, which is in agreement with the solubility of the active compound in ethanol. CONCLUSIONS The conclusions of this study demonstrate that most of these plant extracts should be used with care, especially those which are used with medicinal purposes. This is the first research on the quantification of NDG using MEKC in jarilla extracts.