Search results for "Detection limit"
showing 10 items of 810 documents
Rapid microwave assisted hydrolysis of formetanate
1993
Abstract A fast microwave-assisted hydrolysis procedure has been developed for the derivatization of formetanate previously to the flow-injection spectrophotometric determination of m -aminophenol by reaction with p -aminophenol. Formetanate is quantitatively hydrolyzed with 0.1 M NaOH in 150 s using a closed polyetrafluoroethylene reactor with 115 ml internal volume and a radiation power of 390 W. The above procedure has been applied, as a previous step, for the flow-injection spectrophotometric determination of formetanate in spiked water samples and accurate and precise results have been found. The method permits to obtain a limit of detection of 0.025 mg 1 −1 of formetanate. The relativ…
A rapid and reliable size-exclusion chromatographic method for determination of kojic dipalmitate in skin-whitening cosmetic products
2007
A size-exclusion chromatographic method has been developed to determine the relatively novel skin-whitening agent called kojic dipalmitate (KDP) in skin-whitening cosmetic products. Preliminary experiments were carried out in order to select the solvent for standard and sample solution, and also for mobile phase composition. A PLGel Mixed-D (polystyrene/divinylbenzene co-polymer) column and isocratic mobile phase of pure tetrahydrofuran (at 1.5 mL min(-1) flow rate) were used. Detection was carried out by means of an UV/vis spectrometry detector set at 248 nm. A study of interferences reveals that KDP can be determined without interferences coming from cosmetic matrices. Most other cosmetic…
Extractive-spectrophotometric determination of amphetamine in urine samples with sodium 1,2-naphthoquinone 4-sulphonate
1993
Abstract Sodium 1,2-naphthoquinone 4-sulphonate (NQS) was tested as a reagent for amphetamine in order to develop an extractive-spectrophotometric method for the drug in urine samples. The standard additions method showed the absence of proportional bias error whereas the Youden method and the two standard addition plots method showed the presence of a constant bias error [total Youden blank (TYB)]. Acceptable results were obtained by evaluating the TYB error or by using a placebo (urine sample from a normal subject). The dynamic range of concentrations was 1.4–50 mg 1−1 in urine samples and the detection limit was 0.6 mg 1−1 when 10 ml of urine sample were taken.
Determination of catecholamines as aminochromes by micellar liquid chromatography with thermal lens spectrophotometric detection
1994
The determination of catecholamines (CAs) using micellar liquid chromatography with thermal lens spectrophotometric detection has been studied. CAs are oxidized with hexacyanoferrate(III) to aminochromes which are separated with a mobile phase of 0.05 M sodium dodecyl sulphate, 7% propanol and 0.03 M citrate buffer, pH 4.8, on a partially endcapped C18 column. The aminochrome-micelles and aminochrome-stationary phase association constants are evaluated. Using the 488 nm line of an Ar+ laser with 250 mW pump power the limits of detection are about 4 ng mL−1. The technique is applied to the determination of unconjugated CAs in urine using isoproterenol as internal standard.
HPLC determination of oxadiazon in commercial pesticide formulations
2008
A simple, fast and precise high performance liquid chromatographic (HPLC) procedure has been developed for the determination of oxadiazon in emulsifiable concentrated pesticide formulations. 20 µL of diluted sample in acetonitrile were injected in a Kromasil C18 (250 ×am injetados em uma coluna Kromasil C18 4.6 mm, 5 µm) column, using acetonitrile:water (80:20) as mobile phase at 1 mL min-1 flow rate and oxadiazon determined by absorbance measurement at 292 nm. A theoretical limit of detection of 0.02 µg mL-1, a limit of quantification of 0.047 µg mL-1, corresponding to a 0.02 and 0.07% m/v in the original sample, and a relative standard deviation of 0.08% for three replicate analysis of sa…
Determination of inorganic species by thermal lens spectrometry
1997
Abstract The application of thermal lens spectrometry (TLS) to the determination of inorganic species is reviewed. The requirements of a chromogenic reaction to be advantageously adapted to TLS detection, and the necessary conditions for reaching very low limits of detection are discussed. Methods for the determination of metals and P, Si, S and N compounds in several samples are examined. Flow-injection and extraction methods, associated photoinduced reactions and surface phenomena, speciation and equilibrium studies are discussed. Gas phase NO 2 methods are also commented upon. Trends are given.
DETECTION LIMITS FOR NATURAL CIRCULAR-DICHROISM OF CHIRAL COMPLEXES IN THE X-RAY RANGE
1993
Whereas both Magnetic Circular Dichroism and Faraday Rotation studies have been successfully carried out at the K-, L- and M-absorption edges of metal atoms in ferromagnetic systems, Natural optical activity of chiral complexes has not yet been detected quite unambiguously in the X-ray range. We review a number of theoretical arguments which confirm that the optical asymmetry factor gσ should be very small in the X-ray range for unoriented powdered samples, especially at the K-absorption edges. This stimulating challenge prompted us to start an intensive programme of measurements aimed at detecting natural circular dichroism in both the soft and “firm” X-ray ranges. Although some of our ex…
Matrix solid-phase dispersion extraction procedure for multiresidue pesticide analysis in oranges.
1996
A multiresidue extraction method based on matrix solid-phase dispersion (MSPD) is optimized for the extraction and gas chromatographic screening of eighteen insecticides (aldrin, carbophenothion, captafol, chlorpyriphos, chlorfenvinphos, diazinon, dicofol, alpha-endosulfan, beta-endosulfan, ethion, fenitrothion, folpet, methidathion, malathion, methyl-azinphos, methyl-parathion, phosmet, and tetradifon) from oranges. After optimization of different parameters, such as type of solid phase used and the amount of solid phase or eluent, recoveries ranged from 67 to 102% with relative standard deviations ranging from 2 to 10%. The limits of detection, calculated as 3 times the baseline noise ran…
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…
Direct analysis in real-time high-resolution mass spectrometry as a valuable tool for polyphenols profiling in olive oil
2018
A fast and reliable method to characterize the polyphenolic compound profiles in extra virgin olive oil (EVOO) has been developed using direct analysis in real time (DART) and linear ion-trap Orbitrap mass spectrometry (LTQ-Orbitrap-MS). Hydroalcoholic extraction increased speed and reduced matrix effects, and DART-MS/MS ensured accurate analysis. Characterization of polyphenol fingerprinting in EVOO samples takes 2 min. This method exhibited proper linearity (R2 ≥ 0.99) in the range of 5–2500 μg g−1, limit of detection (LOD) of 1.5 μg g−1 (signal-to noise S/N = 3), and limits of quantitation (LOQs) of 5 μg g−1 (S/N = 10) for resveratrol (a polyphenol not detected in olive oil). Six spiked …