Search results for "Extraction"
showing 10 items of 2072 documents
Determination of UV filters in both soluble and particulate fractions of seawaters by dispersive liquid–liquid microextraction followed by gas chroma…
2014
An analytical method to determine the total content (i.e., not only in the soluble fraction but also in the particulate one) of eight commonly used UV filters in seawater samples is presented for the first time. Dispersive liquid-liquid microextraction (DLLME) is used as microextraction technique to pre-concentrate the target analytes before their determination by gas chromatography-mass spectrometry (GC-MS). In order to release the UV filters from the suspended particles an ultrasound treatment is performed before DLLME. The ultrasound treatment time was studied in order to achieve a quantitative lixiviation of the target analytes. The type and volume of both disperser and extraction solve…
Advantages of monolithic over particulate columns for multiresidue analysis of organic pollutants by in-tube solid-phase microextraction coupled to c…
2011
Abstract The performance of a monolithic C 18 column (150 mm × 0.2 mm i.d.) for multiresidue organic pollutants analysis by in-tube solid-phase microextraction (IT-SPME)-capillary liquid chromatography has been studied, and the results have been compared with those obtained using a particulate C 18 column (150 mm × 0.5 mm i.d., 5 μm). Chromatographic separation has been carried out under isocratic elution conditions, and for detection and identification of the analytes a UV-diode array detector has been employed. Several compounds of different chemical structure and hydrophobicity have been used as model compounds: simazine, atrazine and terbutylazine (triazines), chlorfenvinphos and chlorp…
Improving analysis of apolar organic compounds by the use of a capillary titania-based column: Application to the direct determination of faecal ster…
2010
This article reports a new procedure for the direct determination of faecal sterols coprostanol and cholesterol in wastewater samples as tracers of human sewage contamination. The method combines in-tube solid-phase microextraction (IT-SPME) for analyte enrichment and capillary liquid chromatography (LC) for separation with diode array detection for identification and quantification. A titania-based polymeric capillary column and a conventional octadecyl silica (ODS) capillary column were evaluated and compared for their ability to separate the analytes. The titania-based column allowed the separation of the analytes in much shorter chromatographic times and with better chromatographic prof…
Development of a fully automated sequential injection solid-phase extraction procedure coupled to liquid chromatography to determine free 2-hydroxy-4…
2010
Abstract 2-Hydroxy-4-methoxybenzophenone and 2-hydroxy-4-methoxybenzophenone-5-sulphonic acid, commonly known as benzophenone-3 (BZ3) and benzophenone-4 (BZ4), respectively, are substances widely used as UV filters in cosmetic products in order to absorb UV radiation and protect human skin from direct exposure to the deleterious wavelengths of sunlight. As with other UV filters, there is evidence of their percutaneous absorption. This work describes an analytical method developed to determine trace levels of free BZ3 and BZ4 in human urine. The methodology is based on a solid-phase extraction (SPE) procedure for clean-up and pre-concentration, followed by the monitoring of the UV filters by…
Spectrophotometric determination of phenols in water samples by the GHPSAM method
2001
Abstract The generalized H-point standard-additions method (GHPSAM) is proposed in order to obtain the phenol concentration in water samples when the matrix is completely unknown. The procedure involves solid-phase extraction in BondElut PPL cartridges and data handling of the UV-visible spectrophotometry measurements. The spectral regions where the unknown interferent behaviour can be considered as linear are found and the analyte concentration free from bias error is estimated. The percentages of recovery of phenols in spiked samples were similar to those obtained by HPLC. Cresols or chlorophenols can be also determined in real samples by this method. The concentration range tested was 0.…
Exploring hand-portable nano-liquid chromatography for in place water analysis: Determination of trimethylxanthines as a use case.
2020
Abstract Analytical performance and optimization of figures of merit of a portable nano liquid chromatograph (NanoLC) with UV detection at 255 nm have been established for in place analysis. Methylxanthines: caffeine, theophylline and theobromine were selected as target analytes. A fast lab method based on IT-SPME coupled on line with capillary liquid chromatograph (CapLC) with diode array detection (DAD) was employed for comparative studies. IT-SPME and solid phase extraction were coupled off-line to NanoLC for improving instrumental parameters, mainly detection capacity and selectivity. IT-SPME or SPE/portable NanoLC based methods were superior in terms of chromatographic resolution and o…
Stir bar sorptive-dispersive microextraction mediated by magnetic nanoparticles-nylon 6 composite for the extraction of hydrophilic organic compounds…
2016
A new and sensitive analytical method based on the recently developed approach termed stir bar-sorptive dispersive microextraction (SBSDME) using a magnetic CoFe2O4@SiO2-nylon 6 composite as sorbent material is presented for the extraction of hydrophilic organic compounds. The simultaneous determination of four hydrophilic UV filters in environmental water samples has been chosen as a model analytical application due to the increasing awareness regarding the occurrence of sunscreen residuals in natural waters. The developed SBSDME approach combines the principles and benefits of stir bar sorptive extraction (SBSE) and dispersive solid phase extraction (DSPE) but allows for lower extraction …
A new selective method for dimethylamine in water analysis by liquid chromatography using solid-phase microextraction and two-stage derivatization wi…
2005
Abstract A new method is presented for the determination of DMA in water as its 9-fluorenylmethyl chloroformate (FMOC) derivative using solid-phase microextraction (SPME) and liquid chromatography. The method is based on the employment of SPME fibres coated with carbowax-templated resin (CW-TR) for analyte extraction and derivatization. The fibres were successively immersed in the samples, in a solution of o -phthalaldialdehyde and N -acethyl- l -cysteine (OPA–NAC) and finally, in a solution of FMOC. OPA–NAC reacted on the fibre with possible primary aliphatic amines present in the samples, particularly with PA which is a direct interferent in the determination of DMA with FMOC. In such a w…
Microwave-assisted saponification of animal greases for cholesterol determination
1998
Abstract An alternative method for the hydrolysis of cholesterol esters in animal grease samples has been developed. The method consists of the microwave-assisted treatment of 4 g of animal fat or oil with 40 ml of an ethanolic KOH solution inside a 115 ml closed reactor in which samples were irradiated for 2.5 min at 50% power level of an exit power of 700 W. After extraction with petroleum ether and dissolution of the unsaponifiables in toluene, total cholesterol was determined spectrophotometrically by using p-anisidine as a test reagent of the enzymatic reaction of cholesterol through a bienzymic reactor in which cholesterol oxidase and horseradish peroxidase were noncovalently immobili…
Determination of phenolic antioxidants in vegetal and animal fats without previous extraction by dilution with n-propanol and micellar liquid chromat…
1999
Abstract A simple and rapid HPLC method for the determination of phenolic antioxidants (propyl and octyl gallates, tert -butylhydroquinone and 3- tert -butyl-4-hydroxyanisole) in sunflower, corn and olive oils, margarine, lard and butter oil is described. The samples are diluted with n -propanol, filtered and injected; solutions containing 30% (w/w) sample can be injected. The analytes are separated with a C18 column and a micellar mobile phase containing 0.1 M SDS, 2.5% n -propanol and 10 mM phosphate of pH 3, and detected at 290 nm. Calibration curves are linear ( r > 0.9999) and the limits of detection range from 0.2 to 1.3 ng, which correspond to antioxidant concentrations well below t…