0000000000170776
AUTHOR
M. C. Pascual-martí
Supercritical fluid extraction and high performance liquid chromatography determination of homosalate in lipsticks
Supercritical fluid extraction of homosalate is reported for the first time. Extraction parameters such as pressure, time of extraction, use of modifier, temperature and sample mass were studied. The proposed method was assayed for the extraction of homosalate in sunscreen lipsticks. Efficient recoveries were obtained after 5 min of dynamic extraction with supercritical CO2 and 15% ethanol as modifier at 300 bar and 60°C, flow rate 4 mL min−1. Extracts were dissolved in ethanol, and homosalate determined by HPLC using water—acetic acid—ethanol mobile phase and flow rate of 1 mL min−1. UV detection was at 309 nm using homosalate in ethanol solutions as standards, limit of detection 4 μg mL−1…
Simultaneous determination of oxybenzone and 2-ethylhexyl 4-methoxycinnamate in sunscreen formulations by flow injection-isodifferential derivative ultraviolet spectrometry
Abstract A flow injection procedure was developed for the simultaneous determination of two UV filters (oxybenzone and 2-ethylhexyl 4-methoxycinnamate) in sunscreen formulations, based on the isodifferential approach. The use of the second derivative spectra allowed a selective determination of the analytes free from matrix interferences and without pretreatment of samples. Standard solutions of the analytes were analyzed by the proposed procedure in order to select the appropriate wavelengths to solve the mixture. After this, the procedure was validated using commercial sunscreen formulations the concentrations of which were determined by an HPLC procedure. The two procedures gave comparab…
Determination of selenium, zinc and cadmium in antidandruff shampoos by atomic spectrometry after microwave assisted sample digestion
Microwave assisted pre-treatments for atomic spectrometric determination (inductive coupled plasma-optical emission spectrometry, ICP-OES or flame atomic absorption spectrometry, FAAS) of metallic elements, usually present in antidandruff shampoos, are proposed. They are based on the digestion of the sample with HNO(3) into a closed reactor, which is irradiated at 800 W for a few minutes. Selenium was determined by ICP-OES. The limit of detection was 0.11 mg l(-1); the relative standard deviation (R.S.D.) for the selenium content in the samples was in the 0.6-3.6% range. The results obtained were in agreement with the label contents and the recovery of the proposed method was in the 100-106…
Sequential injection spectrophotometric determination of oxybenzone in lipsticks
A sequential injection (SI) procedure for the spectrophotometric determination of oxybenzone in lipsticks is reported. The colorimetric reaction between nickel and oxybenzone was used. SI parameters such as sample solution volume, reagent solution volume, propulsion flow rate and reaction coil length were studied. The limit of detection was 3 microg ml(-1). The sensitivity was 0.0108+/-0.0002 ml microg(-1). The relative standard deviations of the results were between 6 and 12%. The real concentrations of samples and the values obtained by HPLC were comparable. Microwave sample pre-treatment allowed the extraction of oxybenzone with ethanol, thus avoiding the use of toxic organic solvents. E…
Determination of UV-filters in sunscreens by HPLC.
Simultaneous determination of six internationally authorised organic UV-filters in sunscreen formulations was performed by HPLC with UV spectrophotometric detection. The filters determined were: sulisobenzone, oxybenzone, octyl dimethyl PABA, octyl methoxycinnamate, octyl salicylate and homosalate. A C18 stationary phase and a mobile phase of ethanol water acetic acid (70 : 29.5 : 0.5) were used with a flow rate of 0.5 mL/min. UV measurements were carried out at 313 nm. The time required for the analysis was 25 min and the limits of detection were between 0.2 and 2 mg/L, except for sulisobenzone, which gave a limit of detection of 20 mg/L. The procedure proposed provides an accurate, fast a…
Determination of the UV filters worldwide authorised in sunscreens by high-performance liquid chromatography
Simultaneous determination of organic UV filters worldwide authorised in sunscreen formulations was performed by HPLC with UV spectrophotometric detection. The filters determined were: benzophenone-4, benzophenone-3, butyl methoxydibenzoylmethane, octyl dimethyl PABA, octyl methoxycinnamate, homosalate and octyl salicylate. A C18 stationary phase and an isocratic mobile phase of ethanol-water-acetic acid (70:29.5:0.5) containing 65.4 mM of hydroxypropyl-beta-cyclodextrin, were used with a flow-rate of 0.6 ml/min. UV measurements were carried out at 313 nm. The time required for the analysis was 20 min and the limits of detection were between 1.5 and 2.3 mg/l. The procedure proposed provides…
Identification and determination of amphetamine and methamphetamine in street drugs
Abstract A procedure to identify and quantify amphetamine and/or methamphetamine in street drugs is proposed. The procedure is based on the application of the ACC method (Apparent content curves method) to emission and absorption data of samples. Discrimination and quantification of amphetamine and methamphetamine in samples is carried out based on their different behavior in acid and basic medium. Potential interfering drugs are tested and the accuracy of the method is verified in prepared and real samples. Results obtained are in agreement with a HPLC procedure used as reference.
Supercritical fluid extraction of resveratrol from grape skin of Vitis vinifera and determination by HPLC
Supercritical fluid extraction of resveratrol from grape skin of Vitis vinifera was studied. Extraction variables such pressure, modifier concentration (ethanol), and extraction time were optimised. Final extraction conditions were: 40 degrees C, 150 bar, 7.5% ethanol and extraction time 15 min. Extraction recovery and precision (variation coefficient between 0.2 and 1.0%) were calculated. The resveratrol content in the ethanolic extract was determined by HPLC with UV detection at 306 nm. Acetic acid-methanol-water was used as the mobile phase, and C-18 and C-8 columns were tested, instrumental parameters were optimised, and analytical parameters were calculated (lineal interval 0-75 mg l(-…
Fluorimetric determination of amphetamine in urine by flow injection with on-line liquid–liquid extraction
Abstract Determination of amphetamine in urine was performed by batch and flow injection methodologies. The suitable experimental conditions for fluorimetric measurements were established. The liquid–liquid extraction was carried out at pH 13 using diethyl ether as extracting reagent. The measurement conditions were 260 nm and 277 nm for excitation and emission wavelengths, respectively. The method requires standard addition calibration and Youden blank correction. The influence of the main metabolites of amphetamine and metamphetamine were studied. The accuracy and precision of the proposed method was tested and the method is adapted to the flow injection procedure with on-line extraction.
The linear absorbances method adapted to systems with two interfering compounds
The paper exposes the theoretical and experimental study performed with the purpose to extend the application of the Linear Absorbances Method to more complex systems, which present two spectral interferences. The curves of collinearity are developed and a theoretical study of them is carried out. The theoretical equations developed are experimentally tested and the influence of the variables involved in the Linear Absorbance Method is studied, too. It is concluded that the use of couples of collinear wavelengths of the interferents allows to obtain the concentration of a compound in the presence of two interfering substances.
Efficient flow injection and sequential injection methods for spectrophotometric determination of oxybenzone in sunscreens based on reaction with Ni(II).
Spectrophotometric determination of a widely used UV-filter, such as oxybenzone, is proposed. The method is based on the complexation reaction between oxybenzone and Ni(II) in ammoniacal medium. The stoichiometry of the reaction, established by the Job method, was 1:1. Reaction conditions were studied and the experimental parameters were optimized, for both flow injection (FI) and sequential injection (SI) determinations, with comparative purposes. Sunscreen formulations containing oxybenzone were analyzed by the proposed methods and results compared with those obtained by HPLC. Data show that both FI and SI procedures provide accurate and precise results. The ruggedness, sensitivity and LO…
Determination of essential metals in complete diet feed by flow injection and flame atomic absorption spectrometry
A prior study of different sample pre-treatments for the determination of metallic elements in complete diet feeds was performed in order to choose the most suitable for these samples. The studied pre-treatment were: acid extraction (lixiviation), wet digestion (on microwave oven) and dry ashing mineralization (calcination). Lixiviation (acid extraction) with hydrochloric acid was selected due to its accuracy, fast and simple pre-treatment procedure. Due of the different levels of concentration of the metallic elements in the samples, the same manifold was used but with small variations. Copper (with on-line pre-concentration by chelating Chelex-100 resin), calcium (with on-line dilution) a…
Analytical methodologies for atomic spectrometric determination of metallic oxides in UV sunscreen creams.
In this study, methodologies for determining titanium oxide, zinc oxide and iron oxide are proposed and assayed in commercial sunscreen products. The proposed methodology for TiO2, determination in sunscreens is based on a microwave-assisted treatment for digesting the organic components in a closed teflon reactor in presence of HNO3 and HCl. Titanium is determined by inductive coupled plasma emission spectrometry (ICP-AES). The proposed methodologies for measuring ZnO and Fe2O3 are based on a sample emulsification in water with a non ionic tensioactive and IBMK, followed by Zn and Fe determination by flame atomic absorption spectrometry (FAAS). The methodologies allow a precise and accurat…
Determination of trimethoprim by the linear absorbances method
The determination of trimethoprim in the presence of dyphylline, proxyphylline, theophylline and caffeine by the linear absorbances method is described. Collinear couples of wavelengths, for the interfering dyphylline-proxyphylline-theophylline-caffeine system (in H2SO4, 0.05 mol/L), are provided in order to allow the determination of the analyte in the presence of these interfering substances.
Determination of one compound in the presence of a single interference. Linear absorbances method
The paper exposes the theoretical and experimental principles of an analytical procedure for the determination of one compound in the presence of another with an overlapping absorption spectrum, without the need to use any standard solutions of the latter. The proposed method was applied to the determination of binary mixtures of known composition in order to assess its accuracy and precision.