Search results for "high-performance liquid chromatography"
showing 10 items of 629 documents
A rapid procedure for the determination of caffeine, theophylline and theobromine in urine by micellar liquid chromatography and direct sample inject…
1995
Abstract A liquid chromatographic procedure for the determination of caffeine, theophylline and theobromine in urine samples is described. The proposed system uses a Spherisorb octadecyl-silane ODS-2 C18 analytical column and a guard column of similar characteristics. The UV detector was set at 273 nm. A study to adequately select the composition of the micellar mobile phase for the separation of these compounds in urine samples is performed. Maximum resolution was achieved with a 0.075 M sodium dodecylsulphate-1.5% propanol eluent. Limits of detection at 273 nm ranged between 0.4 μg/ml for theobromine and theophylline and 1.2 μg/ml for caffeine. The procedure allows the determination of th…
High-performance liquid chromatographic determination of tocopherols in infant formulas
2002
A method for the simultaneous determination of alpha-tocopherol acetate and alpha-, delta-, and gamma-tocopherols by normal-phase high-performance liquid chromatography (HPLC) with a fluorescent detector in infant formula is proposed. The values obtained in the determination of the analytical parameters: linearity, precision, limit of detection and accuracy (analysis of a standard reference material, SRM 1846), confirm the quality of the method. The proposed method is useful for the determination of alpha-, delta-, and gamma-tocopherols and alpha-tocopherol acetate in infant formulas at a low cost and in a total time of 2 h.
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/…
Quantitative determination of moniliformin in vegetable foods and feeds
1984
A suitable and simple method for the quantitative determination of moniliformin in vegetable foods and feeds is described. The mycotoxin was extracted by Soxhlet extraction with methanol from mouldy maize, rice, rye, oats, wheat and barley samples. Moniliformin was determined by thin-layer chromatography (TLC) using N-methylbenzthiazolon-2-hydrazone (MBTH) as a new derivatization reagent for this mycotoxin. The moniliformin derivative was assayed at 518 nm. Quantification could be performed after calibration. A linear relationship between mycotoxin amount and peak area was found from 100 to 400 ng/spot. The detection limit is 75 ng/spot.
Selective determination of ammonium in water based on HPLC and chemiluminescence detection
2005
Abstract A selective and sensitive method has been developed for liquid chromatographic determination of ammonium in water samples. The analyte is derivatized with Dansyl Chloride prior to injection into HPLC. Optimal solution derivatization conditions have been established. The dansyl derivative is separated with the aid of a chromatographic column and post-column mixed with peroxyoxalate (TCPO) and H 2 O 2 in order to perform chemiluminescence detection. The detection limit achieved is 8 μg/L and linear response from 0.027 to 0.750 mg/L of ammonium was obtained. Ammonium ion was determined within 2.4 min under optimum chromatographic conditions. The method is fast, and near 10 derivatized…
Use of micellar mobile phases for the chromatographic determination of clorazepate, diazepam, and diltiazem in pharmaceuticals
2001
An ODS-2 column, a micellar mobile phase of high elution strength containing 0.1M sodium dodecyl sulfate and 3% (v/v) butanol, and ultraviolet detection at 230 nm are used for the determination of either of two benzodiazepines (clorazepate and diazepam) and a benzothiazepine (diltiazem) in pharmaceuticals. The procedure is shown to be competitive against conventional chromatography with methanol-water mobile phases, especially for diltiazem. The composition of the micellar mobile phase is selected using a predictive strategy based on an accurate retention model and assisted by computer simulation. Calibration graphs are linear at least in the 2.5 to 20 microg/mL, 4 to 20 microg/mL, and 5 to…
Univariate near infrared methods for determination of pesticides in agrochemicals
2006
Abstract It has been developed a general strategy for the determination of pesticides in agrochemicals by Fourier transform near infrared (FT-NIR) spectroscopy. The methodology is based on previous extraction of the active principles through sonication with acetonitrile and direct determination by transmission measurements, using glass vials as measurement cells and univariate calibration at selected wavenumbers as a function of the pesticide to be analyzed. Chlorsulfuron, metamitron, iprodione, pirimicarb, procymidone and tricyclazole were used as test molecules and data obtained by FT-NIR for 20 samples containing one of these active principles compare well with those found by reference l…
High-performance liquid chromatography of lactose with evaporative light scattering detection, applied to determine fine particle dose of carrier in …
2005
A method for quantification of the fine particle dose of lactose is described, using a hydrophilic interaction chromatography (HILIC) method and evaporative light scattering detection. The HILIC method used an aminopropyl column and a mobile phase consisting of acetonitril/water (80/20, v/v) for isocratic elution. Sensitive chromatography was obtained using a low concentration of water in the extraction solvent. The detection limit (RSD10%) at an injection volume of 10 microL is 10 microg/mL. Linearity was obtained in the range of 10-80 microg/mL (R(2)0.99). A relative standard deviation (RSD) of 0.5% (N=6) demonstrated good precision of the optimized method.
Fourier transform infrared determination of imidacloprid in pesticide formulations
2004
A simple method has been developed for Fourier Transform Infrared (FTIR) determination of Imidacloprid in pesticide formulations. Samples were diluted with CHCl3 and the FTIR spectra of samples and standards were obtained at a nominal resolution of 4 cm-1 from 4000 to 900 cm-1 accumulating 25 scans. Imidacloprid determination was based on the measure of either peak area from 1577 to 1567 cm-1 or peak height at 1572 cm-1, both corrected using a horizontal baseline defined at 1900 cm-1. The limits of detection achieved, of the order of 9 µg g-1, were appropriate for the determination of Imidacloprid in commercially available formulations. FTIR results were statistically comparable to those fo…
Determination of amitraz and its transformation products in pears by ethyl acetate extraction and liquid chromatography-tandem mass spectrometry.
2008
A method has been developed for identification and quantification of the acaricide amitraz and its transformation products, 2,4-dimethylaniline (DMA), 2,4-dimethylformamidine (DMF) and N-2,4-dimethylphenyl-N-methylformamidine (DMPF) in pears. The analytes were extracted using ethyl acetate and anhydrous sodium sulphate. Analysis was performed by liquid chromatography-electrospray tandem mass spectrometry (LC-ESI-MS/MS) in the positive ion mode using a triple quadrupole (QqQ) instrument. Two precursor-product ion transitions were monitored for each compound in the selected reaction monitoring (SRM) mode. The method was validated with pears taken from the orchard before the amitraz treatment …