Search results for "Chloroform"
showing 10 items of 414 documents
Vibrational Spectrometry Strategies for Quality Control of Procymidone in Pesticide Formulations
2005
Abstract Two vibrational spectrometry–based methodologies were developed for procymidone determination in wettable powdered pesticide formulations. The Fourier‐transform infrared (FTIR) procedure was based on the selective extraction of procymidone by chloroform and determination by peak area measurement between 1451 and 1441 cm−1, using a baseline correction established between 1490 and 1410 cm−1, and a precision of 0.4% and a limit of detection of 0.01% w/w procymidone for a sample mass of 25 mg were obtained. For FT‐Raman determination, the selected conditions were peak area measurement between 1005 and 995 cm−1 Raman shift, with a baseline correction fixed between 1030 and 947 cm−1, and…
Quantification of nortriptyline in plasma by HPLC and fluorescence detection
2009
Abstract A simple, sensitive and specific high-performance liquid chromatography method has been developed for the determination of nortriptyline (NT) in plasma samples. The assay involved derivatization with 9H-fluoren-9-ylmethyl chloroformate (Fmoc-Cl) and isocratic reversed-phase (C 18 ) chromatography with fluorescence detection. The developed method required only 100 μl of plasma sample, deproteinized and derivatized in one step. Calibration curves were lineal over the concentration range of 5–5000 ng/ml. The derivatization reaction was performed at room temperature in 20 min and the obtained NT derivative was stable for at least 48 h at room temperature. The within-day and between-day…
Development of a sensitive method for determining traces of prohibited acrylamide in cosmetic products based on dispersive liquid-liquid microextract…
2020
Abstract According to the European Regulation on cosmetic products, the presence of acrylamide in these consumer products is not allowed due to its mutagenic and potentially carcinogenic effects. Despite this ban, acrylamide might be present in those cosmetic products containing acrylamide-based polymers. However, there is no analytical method for its determination in this type of matrices. Based on this, the development of analytical methods for the determination of acrylamide in cosmetic products is required to guarantee consumer safety. In this work, an analytical method for determining traces of prohibited acrylamide in cosmetic products is presented for the first time. The method is ba…
Fourier transform infrared determination of Fluometuron in pesticide formulations
2003
Abstract A single method has been developed for Fourier transform infrared (FTIR) determination of Fluometuron in pesticide formulations. Samples were ultrasonically shaken with CHCl3 for 5 min and the FTIR spectra of sample extracts and standards were obtained at a nominal resolution of 4 cm−1 from 4000 to 900 cm−1 accumulating 25 scans. Fluometuron determination is based on the measure of peak area from 1342 to 1321 cm−1 corrected using a baseline defined from 1352 to 1294 cm−1. This procedure provided a limit of detection of 6.5 μg g−1, a sensitivity of 0.852 a.u. g mg−1 for a pathlength of 0.11 mm, a relative standard deviation of 1.6% for three analysis of a sample containing 50.4% (w/…
In situ derivatization for double confirmation of 2C–C in oral fluids by ion mobility spectrometry
2017
Ion mobility spectrometry (IMS) is a powerful tool to carry out quick and sensitive detection of illicit activities and has been employed for the determination of the psychedelic drug 2,5-dimethoxy-4 chlorophenethylamine (2C–C) in oral fluid samples. Saliva samples were extracted with chloroform and analysed by IMS reaching a limit of detection (LOD) of 14 μg L−1. Nevertheless, IMS has a scarce resolution and selectivity of the method can be often compromised by the presence of potential interferents with similar molecular weights and drift times. Thus, a rapid and in situ derivatization with acetone, to form the corresponding imine, has been proposed in the present study to confirm the pre…
Automated on-line in-tube solid-phase microextraction-assisted derivatization coupled to liquid chromatography for quantifying residual dimethylamine…
2008
Abstract A method for the analysis of dimethylamine (DMA) by automated in-tube solid-phase microextraction (IT-SPME)-supported chemical derivatization coupled with high-performance liquid chromatography was developed. Extraction, derivatization and desorption were studied by using a capillary coated with 95% polydimethylsiloxane and 5% polydiphenylsiloxane. Solution derivatization and automated IT-SPME derivatization using 9-fluorenylmethyl chloroformate (FMOC) were compared. The proposed procedure provided adequate linearity, accuracy and precision in the 0.2–2.0 μg/mL concentration interval, and the limit of detection (LOD) was 50 ng/mL. The main advantages of the proposed procedure are: …
Derivatization of tertiary amphetamines with 9-fluorenylmethyl chloroformate for liquid chromatography: determination of N-methylephedrine.
2000
The fluorogenic reagent 9-fluorenylmethyl chloroformate (FMOC) was evaluated for the derivatization of tertiary amphetamines prior to liquid chromatographic analysis. Conditions for the derivatization were investigated, including the reaction time, the derivatization reagent concentration and the pH, using N-methylephedrine as a model compound. On the basis of these studies, a method for the quantification of N-methylephedrine is presented. The method involves derivatization with FMOC at ambient temperature and separation of the derivatives formed on a LiChrospher C18, 5 μm, 125 × 4 mm id column using acetonitrile–water gradient elution. The proposed procedure shows good linearity, accuracy…
Liquid chromatographic determination of trimethylamine in water.
2004
A method for the selective determination of trimethylamine (TMA) in aqueous matrices by liquid chromatography is reported. The proposed procedure is based on the derivatization of the analyte with 9-fluorenylmethyl chloroformate (FMOC) in a precolumn (Hypersil C18, 30 microm, 20 mm x 2.1 mm i.d.) connected on-line to the analytical column (LiChrosphere 100 RP18, 5 microm, 125 mm x 4 mm i.d.). Gradient elution was performed with a mixture of acetonitrile-water-0.05 M borate buffer (pH 9.0). The method has been applied to the direct determination of TMA in water within the 0.25-10.0 microg/ml concentration interval, and can also be adapted to the determination of TMA over the range 0.05-1.0 m…
FTIR determination of Aspartame and Acesulfame-K in tabletop sweeteners.
2004
Two different strategies for sweeteners determination in tabletop samples by Fourier transform middle-infrared (FTIR) spectrometry, an off-line and a fully mechanized extraction of Aspartame and Acesulfame-K with different mixtures of chloroform and methanol, have been developed. The off-line method involves the extraction of both active principles by sonication of samples with 25:75 v/v CHCl3/CH3OH and direct measurement of the peak height values at 1751 cm(-1), corrected using a baseline defined at 1850 cm(-1) for Aspartame, and measurement of the peak height at 1170 cm(-1) in the first-order derivative spectra, corrected by using a horizontal baseline established at 1850 cm(-1), for Aces…
Sensitive determination of methylenedioxylated amphetamines by liquid chromatography.
2001
Different strategies for the liquid chromatographic determination of methylenedioxylated amphetamines were evaluated: separation and detection of underivatized analytes by (i) UV or (ii) fluorescence, (iii) derivatization with 3,5-dinitrobenzoyl chloride followed by separation and UV detection of the derivatives formed and (iv) derivatization with 9-fluorenylmethyl chloroformate (FMOC) and subsequent separation and fluorimetric detection of the derivatives. The compounds tested were 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxymethamphetamine (MDMA) and 3,4-methylenedioxyethylamphetamine (MDE). On the basis of these studies, a new procedure for the chromatographic determination of…