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showing 10 items of 2807 documents
Spectrophotometric estimation of bicalutamide in tablets
2007
A simple, sensitive, rapid, accurate and precise spectrophotometric method has been developed for the estimation of bicalutamide in bulk and pharmaceutical dosage forms. Bicalutamide shows maximum absorbance at 272 nm with molar absorptivity of 2.3399×10(4) l/mol/cm. Beer's law was obeyed in the concentration range of 1.5-18 μg/ml. The limit of detection and limit of quantification were found to be 0.1 and 0.4 μg/ml, respectively. Results of analysis were validated statistically and by recovery studies.
On-line preconcentration strategies for analyzing pesticides in fruits and vegetables by micellar electrokinetic chromatography.
2007
Five pesticides (fludioxonil, procymidone, pyriproxyfen, dinoseb and carbendazim) were separated in reversed migration micellar electrokinetic chromatography (RM-MEKC) using 20 mmol l(-1) phosphate buffer at pH 2.3, containing 25 mmol l(-1) sodium dodecylsulfate and 10% methanol. Three on-line concentration strategies, sweeping (SW), normal stacking with reversed migration and a water plug (SRW) and stacking with reverse migration and removal of sample matrix using polarity switching (SRMM), were compared. About 10-, 30- and 50-fold increases in detection sensitivity, compared with standard hydrodynamic injection (5 s at 0.5 psi), were observed with SW, SRW and SRMM, respectively. Limits of…
Non-chromatographic speciation of toxic arsenic in vegetables by hydride generation-atomic fluorescence spectrometry after ultrasound-assisted extrac…
2007
A non-chromatographic, sensitive and simple analytical method has been developed for the determination of toxic arsenic species in vegetable samples by hydride generation-atomic fluorescence spectrometry (HG-AFS). As(III), As(V), dimethylarsinic acid (DMA) and monomethylarsonic acid (MMA) were determined by hydride generation-atomic fluorescence spectrometry using a series of proportional equations. The method is based on a single extraction of the arsenic species considered from vegetables through sonication at room temperature with H(3)PO(4) 1 mol L(-1) in the presence of 0.1% (w/v) Triton XT-114 and washing of the solid phase with 0.1% (w/v) EDTA, followed by direct measurement of the co…
Identification of lipid binders in old oil paintings by separation of 4-bromomethyl-7-methoxycoumarin derivatives of fatty acids by liquid chromatogr…
2005
A HPLC-fluorescence method for identification of drying oils from binding media or protective film used in pictorial works of art prior to conservation or restoration is proposed. Fluorescence derivatization of fatty acids released by hydrolysis of structural drying oils is studied. The derivatization reagent was 4-(bromomethyl)-7-methoxycoumarin with 18-crown-6 as catalyst. Mobile phase was programmed from methanol-water (90:10 v/v) to methanol-water (100:0 v/v) in 25 min. The excitation and emission wavelengths were 325 and 395 nm, respectively. Under these chromatographic conditions, coumarin derivatives of myristic, palmitic, oleic and stearic acids were satisfactorily resolved. The met…
Recent developments in isotope ratio measurements by resonance ionization mass spectrometry
2005
Resonance ionization mass spectrometry (RIMS) has become a sensitive and highly selective technique for the determination of extremely low elemental or isotopic abundances, involving isotope ratio measurements with dynamical ranges of 109 and beyond. The experimental detection limits are as low as 106 atoms per sample, and isotopic selectivities of up to 1013 have been achieved under optimal conditions. The potential of RIMS using different experimental systems is outlined in the determination of lowest abundances and isotope ratios of long-lived radioisotopes of general importance like Pu238–244, 41Ca, and 236U for studies in geosciences, environmental, bio-medical or fundamental research.
Determination of ascorbic acid in asparagus by differential pulse polarography
1995
A useful method for the determination of ascorbic acid in a vegetable product (asparagus) by differential pulse polarography has been set up and evaluated. Extraction and instrumental conditions were optimized. The analytical parameters are: linearity (0–18.18 μg/ml); detection limit (0.182 μg/ml); instrumental and method precision (2.77% and 4%, respectively); accuracy (96.9–113.4%). These data show that the method is sufficiently sensitive, reliable and accurate. It was also compared with the official fluorometric AOAC method.
Quality control of pharmaceuticals containing clenbuterol by thermal lens spectrometry.
1996
An ultrasensitive absorptiometric procedure for the determination of clenbuterol in pharmaceutical preparations was developed. Clenbuterol was diazotized with nitrite and coupled with 1-(naphthyl)ethylenediamine, and the absorbance of the azo dye formed was measured by both spectrophotometry and ultrasensitive thermal lens spectrometry (TLS). The TLS limit of detection was 1.5 ppb, 14-fold lower than with a Hewlett-Packard diode array spectrophotometer. Thus, the TLS procedure can be advantageously applied to quality control of clenbuterol at the individual dose level and in small samples. Repeatability as relative standard deviation was 1.5% (50 ppb, n = 6).
Analysis of thiabendazole and procymidone in fruits and vegetables by capillary electrophoresis–electrospray mass spectrometry
2002
Abstract A capillary electrophoresis–mass spectrometry method for determining procymidone and thiabendazole in apples, grapes, oranges, pears, strawberries and tomatoes is described. Separation is achieved using a buffer of formic acid–ammonium formate at pH 3.5 with 2% of methanol. Fungicide residues present in the sample are preconcentrated by both solid-phase extraction and injection of large sample volumes into the capillary by a stacking technique, to obtain lower detection limits. Ionization is performed at atmospheric pressure in an electrospray type source and detection is carried out using positive ionization and selected ion monitoring modes. The quantitation limits are 0.005 and …
Application of stable isotopes and AF4/ICP-SFMS for simultaneous tracing and quantification of iron oxide nanoparticles in a sediment–slurry matrix
2016
One major challenge in nanomaterial analysis, especially in complex environmental matrices, is the unambiguous differentiation between natural and engineered nanomaterials (ENMs). Particularly with regard to the investigation of ENM's/engineered nanoparticle's (ENPs) fate, analytical methods are needed allowing for tracing and sensitive quantification. Several ENPs are metal-based and contain elements being omnipresent in environmental matrices (e.g., Al, Ti, Zn, Fe and non-metal Si) – hence, high background levels of these elements are expected, compromising sensitive detection. In this work we developed successfully a combined approach of stable isotope labeling (tracing) and reverse post…
On-line gel permeation chromatography–attenuated total reflectance–Fourier transform infrared determination of lecithin and soybean oil in dietary su…
2007
Gel permeation chromatography (GPC) with attenuated total reflectance-Fourier transform infrared (ATR-FTIR) spectrometry detection has been proposed for the simultaneous determination of lecithin and soybean oil in dietary supplements. The method involves the extraction of analytes with dichloromethane in an ultrasound water bath and the injection of 2 ml of centrifuged and filtered extracts into the system integrated by two Envirogel GPC columns (19 mm x150 mm, 19 mm x 300 mm) coupled on-line. Dichloromethane was used as mobile phase. A method has been developed to select the most appropriated wavenumber to be used for the determination of each considered compound from the calculation of a…