Search results for "solid phase"
showing 10 items of 360 documents
Gas chromatographic behaviour of urea herbicides
2001
Gas chromatographic conditions for determining eight phenylurea (chlortoluron, diuron, fluometuron, isoproturon, linuron, metabenzthiazuron, metobromuron and monuron) and one sulfonylurea (chlorsulfuron) herbicides were assessed. Degradation products of the herbicides formed in the injector were used for identification. Most phenylureas formed their respective carbamic acid methyl esters, metabenzthiazuron formed an aminobenzothiazol and chlorsulfuron formed an aminotriazine plus a phenylsulfonamide. On-column injection of standards using a BP10 capillary column was evaluated to identify the chromatographic behaviour. Detection limits ranged from 0.05 ng for chlorsulfuron to 3 ng for monuro…
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…
Determination of organophosphorus pesticides in honeybees after solid-phase microextraction.
2001
A method based on solid-phase microextraction (SPME) followed by gas chromatography with nitrogen-phosphorus detection was developed for the purpose of determining 18 organophosphorus pesticide residues in honeybee samples (Apis mellifera). The extraction capacities of polyacrylate and poly(dimethylsiloxane) fibers were compared. The main factors affecting the SPME process, such as the absorption time profile, salt, and temperature, were optimized. The method involved honeybee sample homogenization, elution with an acetone:water solution (1:1) and dilution in water prior to fiber extraction. Moreover, the matrix effect on the extraction was evaluated. In samples spiked at the 0.2 mg kg(-1) …
DETERMINATION OF PENTOBARBITAL IN BIOLOGICAL SAMPLES BY MICELLAR LIQUID CHROMATOGRAPHY
1999
A liquid chromatographic procedure for the determination of pentobarbital in urine and plasma samples is described. The proposed system uses a Spherisorb octadecyl-silane ODS-2 C18 analytical column, a guard column of similar characteristics, and a 0.02 M CTAB-15% 1-propanol at pH 7.5 mobile phase. The UV detector was set at 250 nm. Pentobarbital was isolated from urine and plasma samples by using a single solid phase extraction procedure with LMS cartridges. Mephobarbital was used as internal standard. Limits of detection were 0.53 μg/mL and 0.60 μg/mL in urine and plasma samples respectively. In both cases the coefficients of variation were lower than 6.5%, and the recoveries ranged betwe…
Determination of abamectin in citrus fruits by liquid chromatography-electrospray ionization mass spectrometry.
2000
Liquid chromatography coupled to electrospray mass spectrometry (LC-ES-MS) with positive ion detection was used to determine abamectin in oranges. MS conditions were optimized to achieve maximum sensitivity. The main ion for abamectin was [M+Na]+ at a fragmentor voltage of 180 V. Abundant structural information can be obtained at different fragmentor voltages. The detection limit for the standard solution was 12 pg injected, and good linearity and reproducibility were observed. Abamectin residues were extracted using matrix solid-phase dispersion. Orange samples were homogenized with C18 bonded silica placed onto a glass column and eluted with dichloromethane. Recoveries of the abamectin fr…
Selective and sentivive method based on capillary liquid chromatography with in-tube solid phase microextraction for determination of monochloramine …
2015
Abstract Due to the difficulties of working with chloramines, a critical examination of monochloramine standard preparation has been performed in order to select the best synthesis conditions. The analyte has been determined by in-tube solid phase extraction coupled to capillary liquid chromatography with UV detection (IT-SPME Capillary LC DAD). Potential factors affecting the response of monochloramine such as the pH of mobile phase and the volume of sample processed by IT-SPME Capillary LC DAD have been investigated and optimized. According to the results of the study, 0.1 mL or 4.0 mL of sample at neutral pH were loaded in the chromatographic system. A sensitive and selective method has …
Capillary zone electrophoresis for the determination of thiabendazole, prochloraz and procymidone in grapes
2001
Capillary zone electrophoresis with UV detection was applied to the simultaneous determination of thiabendazole, prochloraz and procymidone in grapes. Electrolyte conditions such as pH, composition and concentration of the buffer, addition of organic solvent and working voltage were checked to obtain a high-performance separation of the three fungicides (by measurement of separation efficiency and resolution). The most critical parameter was the pH of the running buffer. The best separation was achieved in 4 mM phosphate solution at pH 3.5. The repeatability of the migration times, expressed as RSD, was <0.44%. The three peaks were completely resolved with a separation efficiency up to 100 …
Determination of type A and type B trichothecenes in paprika and chili pepper using LC-triple quadrupole-MS and GC-ECD.
2011
There is a need to develop sensitive and accurate analytical methods for determining deoxynivalenol (DON), HT-2 toxin and T-2 toxin in paprika to properly assess the relevant risk of human exposure. An optimized analytical method for determination of HT-2 toxin and T-2 toxin using capillary gas chromatography with electron capture detection and another method for determination of DON by liquid chromatography-mass spectrometry in paprika was developed. The method for determination of HT-2 toxin and T-2 toxin that gave the best recoveries involved extraction of the sample with acetonitrile-water (84:16, v/v), clean-up by solid-phase extraction on a cartridge made of different sorbent material…
Determination of the new psychoactive substance dichloropane in saliva by microextraction by packed sorbent – Ion mobility spectrometry
2018
Abstract A simple procedure based on microextraction by packed sorbent (MEPS) has been proposed for the extraction of dichloropane in oral fluids and its determination by ion mobility spectrometry (IMS). Extraction conditions such as type of sorbent (octyl and octadecyl silica), sample pH, number of sample loadings, and elution volume were evaluated to obtain the most appropriate values. Dichloropane was extracted from saliva samples using C8 MEPS, loading with 100 μL sample (adjusted to pH 7) in 4 cycles, washing with 100 μL deionized water, and eluting with 50 μL 2-propanol in 10 cycles. The proposed MEPS procedure has been validated in terms of linearity, accuracy, and precision. A limit…
Determinación de residuos de paraquat en lechuga y repollo cultivados en Lepaterique mediante HPLC-DAD
2018
La determinación de residuos del herbicida paraquat en lechuga (Lactuca sativa) y repollo (Brassica oleracea) producidos en la comunidad de La Brea, Lepaterique y comercializados en la ciudad de Tegucigalpa fue llevada a cabo en los meses de octubre y noviembre de 2017, mediante la aplicación de cromatografía líquida de elevada resolución con detector de arreglo de diodos (HPLC-DAD) en menos de 6 minutos, con un mecanismo de separación de fase reversa empleando una columna superficialmente porosa C18 y una mezcla de ácido orto fosfórico al 0.1 M (pH 3,0) con acetonitrilo en proporción de 3:1 como fase móvil. El método se basa en la extracción con baño ultrasónico utilizando agua como solven…