Search results for "Chemical analysis"
showing 10 items of 324 documents
Fishing for a drug: solid-phase microextraction for the assay of clozapine in human plasma
1999
Solid-phase microextraction (SPME) was investigated as a sample preparation method for assaying the neuroleptic drug clozapine in human plasma. A mixture of human plasma, water, loxapine (as internal standard) and aqueous NaOH was extracted with a 100-micron polydimethylsiloxane (PDMS) fiber (Supelco). Desorption of the fiber was performed in the injection port of a gas chromatograph at 260 degrees C (HP 5890; 30 m x 0.53 mm I.D., 1 micron film capillary; nitrogen-phosphorous selective detection). Fibers were used repeatedly in up to about 75 analyses. The recovery was found to be 3% for clozapine from plasma after 30 min of extraction. However, in spite of the low recovery, the analyte was…
Determination of atranol and chloroatranol in perfumes using simultaneous derivatization and dispersive liquid-liquid microextraction followed by gas…
2013
Abstract A new analytical method based on simultaneous derivatization and dispersive liquid–liquid microextraction (DLLME) followed by gas chromatography–mass spectrometry (GC–MS), for the determination of the allergenic compounds atranol and chloroatranol in perfumes, is presented. Derivatization of the target analytes by means of acetylation with anhydride acetic in carbonate buffer was carried out. Thereby volatility and detectability were increased for improved GC–MS sensitivity. In addition, extractability by DLLME was also enhanced due to a less polar character of the solutes. A liquid–liquid extraction was performed before DLLME to clean up the sample and to obtain an aqueous sample …
Determination of ruthenium in photographic emulsions - Development and comparison of different sample treatments and mass spectrometric methods
1999
Different sample treatment procedures were combined with inductively coupled plasma mass spectrometry (ICP-MS) and negative thermal ionisation mass spectrometry (NTI-MS) for the determination of ruthenium traces in photographic emulsions. Dissolution of the samples in concentrated ammonia solution was used in connection with ICP-MS by external calibration, which has the advantage of a simple sample preparation technique but introduces high amounts of the silver matrix into the mass spectrometer. On the other hand, isotope dilution mass spectrometry (IDMS) with an enriched 99Ru spike solution was applied for ICP-MS and NTI-MS measurements, respectively, in connection with a significant reduc…
A solid-phase extraction and size-exclusion liquid chromatographic method for polyethylene glycol 25 p-aminobenzoic acid determination in urine: Vali…
2007
No previous publications about percutaneous absorption of polyethylene glycol 25 p-aminobenzoic acid (PEG-25 PABA) have been found in the literature and the expected levels to be found in human urine after sunscreens use are unknown. The method proposed here is suitable to determine PEG-25 PABA in the urine of sunscreens users in order to carry out studies on body accumulation/excretion. It is based on solid-phase extraction (SPE) with size-exclusion liquid chromatography determination. Solid-phase extraction allows the analyte to be retained and subsequently eluted for a clean-up, using a silica-based cartridge. The size-exclusion liquid chromatography of the eluted allows the rest of matr…
Electrochemical detection of uric acid and ascorbic acid using r-GO/NPs based sensors
2021
Abstract A sensitive and selective electrochemical sensor, based on reduced graphene oxide and gold nanoparticles obtained by simple co-electrodeposition, was developed for the detection of uric acid and ascorbic acid. Because of the electrochemical oxidation of both uric and ascorbic acid depending on the pH, the sensor performances were studied at different pH values. Excellent results were obtained for uric acid detection in a linear range from 10 to 500 µmol dm−3 with a sensitivity of 0.31 µA cm−2 µM−1. A limit of detection and quantification of 3.6 µM and 10.95 µmol dm−3, respectively, was calculated. Sensors showed good selectivity toward different interfering species present in the m…
A cost-effective method for estimating di(2-ethylhexyl)phthalate in coastal sediments.
2013
This study describes the development of a new method for the analysis of di(2-ethylhexyl)phthalate (DEHP) using 0.1-0.3 g of sediment sample, based on matrix solid phase dispersion (MSPD) using C18 as dispersant phase (0.4 g) and acetonitrile-water as eluting solvent (3.4 mL 1:3.25, v/v). No evaporation step is required. 3 mL of extracts were processed on-line by in-tube solid phase microextraction (IT-SPME) coupled to capillary liquid chromatography (CapLC) and diode array detector (DAD). A short analytical column Zorbax SB C18 (35×0.5 mm, 5 μm) provided suitable results. FTIR-ATR was employed for characterizing sediment samples and MSPD procedure. The total analysis time was less than 20 …
Rapid screening of organophosphorus pesticides in honey and bees by liquid chromatography—Mass spectrometry
2002
Twenty-two organophosphorus pesticide residues were simultaneously determined in honey and honeybee samples by extraction procedures based on solid-phase and liquid chromatography-atmospheric pressure chemical ionization-mass in positive and negative ionization modes. Pesticides in honeybee samples were extracted by matrix solid phase dispersion with C18 silica and subsequently eluted with a mixture of dichloromethane-methanol (85∶15, v/v). The average recoveries from spiked honeybees (0.5–10 μg g−1) ranged from 76% for coumaphos to 100% for omethoate, with relative standard deviations between 3 and 17%. Limits of detection were ≤0.13 μg g−1 and limits of quantification were ≤0.43 μg g−1. H…
Improving detection limits for organotin compounds in several matrix water samples by derivatization-headspace-solid-phase microextraction and GC-MS.
2010
Triethyltin, tributyltin, diphenyltin and triphenyltin were selected as model compounds. The method is based on in situ ethylation and simultaneous headspace-solid-phase microextraction (HS-SPME) and gas chromatographic-mass spectrometry analysis (GC-MS). The extraction procedure was optimized studying some variables such as reaction time, salinity, sample volume and headspace volume. SPME-GC-MS and SPME-GC-FID techniques were compared; quality assurance parameters such as sensitivity, selectivity and precision were established. The proposed procedure showed limits of detection between 0.025 and 1 ng/L. The linearity was in the 0.025-5000 ng/L range. The precision expressed as relative stan…
Comparison of different methods for extraction of polycyclic aromatic hydrocarbons (PAHs) from Sicilian (Italy) coastal area sediments.
2012
This paper describes a work aimed at improving the conditions of an extraction method, coupling GC-MS determination, for the analysis without cleanup phase, of polycyclic aromatic hydrocarbons (PAHs) from sediment samples. The automatic Soxhlet extraction in warm mode (using Extraction System B-811 Standard, Buchi) has demonstrated advantages for automation, reduced extraction time, and lower solvent use than for conventional Soxhlet extraction. Under these conditions, the recoveries are very good as they resulted greater than 85 % and, in most of the cases, near 100 %. The repeatability is also satisfactory (relative standard deviation less than 15 %). The detection limits are also accepta…
Antibody-Capped Mesoporous Nanoscopic Materials: Design of a Probe for the Selective Chromo-Fluorogenic Detection of Finasteride
2012
[EN] The synthesis of capped mesoporous silica nanoparticles (MSN) conjugated with an antibody (AB) as a gatekeeper has been carried out in order to obtain a delivery system able to release an entrapped cargo (dye) in the presence of a target molecule (antigen) to which the conjugated antibody binds selectively. In particular, MSN loaded with rhodamine B and functionalized on the external surface with a suitable derivative of N-(t-butyl)- 3-oxo-(5a,17b)-4-aza-androst-1-ene-17-carboxamide (finasteride) have been prepared (S1). The addition of polyclonal antibodies against finasteride induced capping of the pores due to the interaction with the anchored hapten-like finasteride derivative to g…