Search results for "Kinetic"
showing 10 items of 3064 documents
Analysis of post-harvest fungicides by micellar electrokinetic chromatography.
2001
A method based on solid-phase extraction (SPE) and micellar electrokinetic chromatography (MEKC) was developed for the simultaneous determination of carbendazim, imazalil, methylthiophanate, O-phenylphenol, prochloraz, procimidone, thiabendazole and triadimefon residues in grape, lettuce, orange and tomato. Selectivity and resolution were studied changing the pH and the concentration of the buffer, the type and concentration of surfactant and the methanol content in the mobile phase. A buffer consisting of 4 mM borate with 75 mM sodium cholate (pH 9.2) gave the best results. The recoveries of the fungicides in spiked fruit and vegetable samples ranged from 30 to 105%, and the limits of dete…
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…
RAPID LIQUID CHROMATOGRAPHIC DETERMINATION OF TETRACYCLINES IN ANIMAL FEEDS USING A SURFACTANT SOLUTION AS MOBILE PHASE
2002
ABSTRACT A chromatographic procedure was developed for the determination of oxytetracycline (OTC), tetracycline (TC), chlortetracycline (CTC), doxycycline (DC) and minocycline (MINO) in animal feeds. Clear analyte-rich extracts were obtained using a 1 : 1 acetonitrile/water mixture buffered at pH 3. The extracts were injected into a conventional unprotected C18 chromatographic column and eluted with a mobile phase of 0.05 M sodium dodecyl sulfate/5% 1-butanol/0.01 M oxalic acid at pH 3. Good resolution was achieved for the five compounds, whereas OTC and TC coeluted with an optimized aqueous-organic mobile phase of methanol/acetonitrile/0.01 M oxalic acid at pH 3. Mean recoveries from spike…
Simultaneous determination of olanzapine, clozapine and demethylated metabolites in serum by on-line column-switching high-performance liquid chromat…
2001
An automated method for simultaneous routine quantification of the antipsychotic drugs clozapine, olanzapine and their demethylated metabolites is described. The method included adsorption on a cyanopropyl (CPS) coated clean-up column (10 microm; 10 x 2.0 mm I.D.), washing off interfering serum constituents to waste, and separation on C18 ODS Hypersil reversed phase material (5 microm; 250 x 4.6 mm I.D.) using acetonitrile-water-tetramethylethylenediamine (37:62.6:0.4, v/v/v) adjusted to pH 6.5 with concentrated acetic acid. UV-detection was performed at 254 nm. The limit of quantification was 10-20 ng/ml. Relative day to day standard variations ranged between 4.5 and 13.5%. The method is s…
Determination of synthetic antioxidants in dairy products and dietetic supplements by micellar liquid chromatography with direct sample injection
2000
A simple and rapid HPLC method for the determination of synthetic antioxidants (propyl gallate, tert-butylhydroquinone, 2,4,5-trihydroxybutyrophenone, nordihydroguaiaretic acid, octyl gallate, 3-tert-butyl-4-hydroxyanisole and dodecyl gallate) in powdered and liquid milk, cream of milk and dietetic supplements is described. The samples are diluted or solved in a micellar solution, filtered and directly injected. The retention behavior of the antioxidants on a C18 column, with micellar mobile phases containing SDS (0.05–0.15 M), n-propanol (1–9%, v/v) and 10 mM phosphate at pH 3, has been studied by using mathematical models. Retention is predicted with errors below 3%. To optimize the mobil…
Determination of furosemide in urine samples by direct injection in a micellar liquid chromatographic system.
2002
A sensitive, selective and efficient micellar liquid chromatographic (MLC) procedure was developed for the determination of furosemide (4-chloro-N-furfuryl-5-sulfamoylanthranilic acid) in urine samples by direct injection and UV detection. The procedure makes use of a C18 reversed-phase column and a micellar mobile phase of 0.05 mol l(-1) sodium dodecyl sulfate-6% v/v propanol and phosphate buffer at pH 3 to resolve furosemide from its photochemical degradation products. The importance of protecting the standards and urine samples to be analysed from light in the assay of furosemide, avoiding its degradation, was verified. The limit of quantification was 0.15 microg ml(-1) and the relative …
MICELLAR LIQUID CHROMATOGRAPHIC DETERMINATION OF ANTI-CONVULSANT DRUGS IN PILLS AND CAPSULES
2000
A simple chromatographic procedure is reported for the determination of several anti-convulsant drugs in pharmaceuticals: carbamazepine, and the benzodiazepines bentazepam, halazepam, oxazepam, pinazepam, and tetrazepam. The procedure utilizes a C18 column, a hybrid micellar mobile phase of 0.1 M SDS-3% butanol-0.1% triethylamine-0.01 M phosphate buffer (pH 3), and UV detection (230 nm). The drugs eluted in less than 13 min, in accordance to their relative polarities, as indicated by their octanol-water partition coefficients. The limits of detection (μg/mL), and intra and inter-day repeatabilities (%), for 4 μg/mL were: carbamazepine (0.03, 1.0, 4.1), bentazepam (0.05, 1.3, 1.6), halazepam…
Automated Determination of Trimipramine and N-Desmethyl-Trimipramine in Human Plasma or Serum by HPLC With On-Line Solid Phase Extraction
1995
A fully automated method including column-switching and isocratic high performance liquid chromatography (HPLC) was developed for determination of the tricyclic antidepressant trimipramine (T) and its N-demethylated metabolite N-desmethyltrimipramine (DT). The limit of quantification was below 10 ng/ml for T and DT. The assay revealed linearity between detector response and drug concentration in a therapeutically relevant range of 10 to 500 ng/ml. The mean intra- and interassay variabilities were 6.2 and 12.3%, respectively, for T and 4.7 and 8.7% respectively, for DT. The method can be applied to therapeutic drug monitoring of patients under T therapy and may be useful for pharmacokinetic …
eta1-Allypalladium complexes with tridentate PNP’ ligand for the assembly of modified Screen Printed Electrodes: an electrochemical study.
2015
Specific Pd-based organometallic complex, in particular the [Pd(η1-CH2–CH=CH2)(P–N–P’)]BF4 was used for the assembly of chemically modified Screen Printed Electrodes (SPEs) and their electrochemical reactivity was also investigated. For this purpose potassium ferricyanide, hexaammineruthenium(III) chloride, sodium hexachloroiridate-(III) hydrate, ascorbic acid (AA), uric acid (UA), acetaminophen (Ac), guanine (G) and adenine (A) were used to study the electron-transfer processes, which occurred at modified SPEs, fabricated by using the [Pd(η1-CH2–CH=CH2)(P–N–P’)]BF4, applying the drop casting procedure. Interesting results were obtained in the case of the guanine (G) quantitative detection,…
A multicommuted flow system with solenoid micro-pumps for paraquat determination in natural waters.
2007
A flow system designed with solenoid micro-pumps is proposed for the determination of paraquat in natural waters. The procedure involves the reaction of paraquat with dehydroascorbic acid followed by spectrophotometric measurements. The proposed procedure minimizes the main drawbacks related to the standard chromatographic procedure and to flow analysis and manual methods with spectrophotometric detection based on the reaction with sodium dithionite, i.e. high solvent consumption and waste generation and low sampling rate for chromatography and high instability of the reagent in the spectrophotometric procedures. A home-made 10-cm optical-path flow cell was employed for improving sensitivit…