Search results for "LIMIT"
showing 10 items of 2826 documents
Determination of clenbuterol in urine by azo-dye precolumn derivatization and micellar liquid chromatography
1997
Clenbuterol has been determined in urine by solidphase extraction on a C18 cartridge, diazotization of the eluate with nitrite, coupling of the diazonium ion with 1-(naphthyl)ethylenediamine, and separation of the azo dye formed by HPLC with a C18 column and a micellar mobile phase containing 0.1 M sodium dodecyl sulphate, 12%n-butanol and 0.05 M citrate buffer, pH 3. Recoveries higher than 90% were obtained by mixing the samples with a 20% 0.2 M NaOH before extraction. Limits of detection of 51 and 6.7 ng L−1 were obtained with spectrophotometric and thermal lens spectrometric detection, respectively; respective repeatabilities were 3.1% (5 μg mL−1) and 5.6% (0.16 μg mL−1).
Determination of catecholamines in urine by micellar liquid chromatography with coulometric detection
1994
The determination of catecholamines by HPLC with a sodium dodecyl-sulphate (SDS), micellar mobile phase on a C18 column and with coulometric detection was studied. The eluate was conditioned at +0.25 and +0.00 V, and the current at −0.16V was recorded. A previously developed model which describes the chromatographic behaviour of solutes in HPLC with hybrid, micellar mobile phases was used to optimize the SDS and ethanol concentrations. A mobile phase of 0.15M SDS in a phosphate buffer of pH 3.4 and without ethanol is recommended. The limits of detection were 0.4–0.7 ng ml−1. The procedure was applied to the determination of unconjugated L-dopa, norepinephrine and dopamine in urine. Direct i…
Flow injection-chemiluminescence determination of octyl dimethyl PABA in sunscreen formulations
2002
Abstract A sensitive flow injection (FI) procedure was developed for the determination of the UV-filter octyl dimethyl PABA in sunscreen formulations based on its chemiluminescence (CL) induced by potassium permanganate in sulfuric acid. Both second-order and log–log calibration graphs can be used to perform the analysis. Ninety injections per hour can be carried out, which means a sample throughput of 18 h −1 if five injections per solution are performed. The limit of detection (3 σ ) was 25 ng ml −1 . The interference effects of the excipient and other UV filters are studied. Sunscreen formulations containing octyl dimethyl PABA were analysed by both the proposed FI-CL method and a liquid…
Simultaneous determination of Folpet and Metalaxyl in pesticide formulations by flow injection Fourier transform infrared spectrometry
2003
Fourier transform infrared (FTIR) spectrometric methodology has been developed for the simultaneous determination of Folpet and Metalaxyl in pesticide formulations. The method involves the extraction of both active principles by sonication of the sample with CHCl3 and direct measurement of the absorbance using peak height values at 1798 cm −1 corrected with a baseline defined at 1810 cm −1 for Folpet, and peak area data established from 1677 to 1667 cm −1 corrected using a baseline from 1692 to 1628 cm −1 for Metalaxyl. Limits of detection (3 s) values of 17 and 16 gg −1 were found for Folpet and Metalaxyl, respectively, with results comparable with those found by liquid chromatography with…
Sequential injection spectrophotometric determination of oxybenzone in lipsticks
2001
A sequential injection (SI) procedure for the spectrophotometric determination of oxybenzone in lipsticks is reported. The colorimetric reaction between nickel and oxybenzone was used. SI parameters such as sample solution volume, reagent solution volume, propulsion flow rate and reaction coil length were studied. The limit of detection was 3 microg ml(-1). The sensitivity was 0.0108+/-0.0002 ml microg(-1). The relative standard deviations of the results were between 6 and 12%. The real concentrations of samples and the values obtained by HPLC were comparable. Microwave sample pre-treatment allowed the extraction of oxybenzone with ethanol, thus avoiding the use of toxic organic solvents. E…
Simultaneous detection of three antiviral and four antibiotic compounds in source-separated urine with liquid chromatography
2013
An analytical method for the simultaneous screening of three antiviral agents (nevirapine, zidovudine, lamivudine), four antibiotics (sulfamethoxazole, trimethoprim, ciprofloxacin, rifampicin) and one reference compound (carbamazepine) in human urine was developed. Separation was achieved with a Kinetex XB-C18 (75 × 4.6 mm, 2.6 μm) column after the extraction of pharmaceuticals from urine with SPE. Gradient elution with a mobile phase consisting of acetonitrile and 10 mM KH2 PO4 (pH 2.5), and diode array detection with monitoring at 210 and 264 nm was applied. The developed method was validated in terms of selectivity, linearity, stability and sensitivity. Repeatability (n = 3) and between-…
Indicator-free electrochemical DNA hybridization biosensor
1998
A new electrochemical hybridization biosensor protocol without an external indicator is described. The biosensor format involves the immobilization of inosine-substituted (guanine-free) probe onto the carbon paste transducer, and a direct chronopotentiometric detection of the duplex formation by the appearance of the guanine oxidation peak of the target. Such a use of the intrinsic DNA electrochemical response for monitoring hybridization events offers several advantages (over the common use of external indicators), including the appearance of a new peak, a flat background, or simplicity. A 4 min short hybridization period allows a detection limit around 120 ng/ml. Performance characteristi…
High performance liquid chromatography—atomic fluorescence spectrometric determination of arsenic species in beer samples
2003
Abstract A method has been developed for the direct determination of As(III), dimethylarsinic acid (DMA), monomethylarsonic acid (MMA) and As(V) in beers by hydride generation—atomic fluorescence spectrometry after separation of arsenic species by high performance liquid chromatography. Compounds were separated by anion-exchange chromatography with isocratic elution using KH 2 PO 4 /K 2 HPO 4 as mobile phase with elution times of 1.67, 2.08, 6.52 and 10.72 min for As(III), DMA, MMA and As(V), respectively. Parameters affecting the hydride generation of all arsenic species were studied and the best conditions were established as a reaction coil of 150 cm, for a sample injected volume of 100 …
Determination of total arsenic in soft drinks by hydride generation atomic fluorescence spectrometry
2007
Abstract A highly sensitive and simple method has been developed for the determination of total arsenic, by continuous hydride generation and atomic fluorescence spectrometry (HGAFS), in refreshing drink samples as colas, teas and fruit juices. Samples were mixed with concentrated HCl and KI to obtain final concentrations of 2 mol l−1 and 1%, respectively. These solutions were aspirated and merged with a reducing NaBH4 3% (m/v) solution, with sample and NaBH4 flow rates of 12.5 and 1.5 ml min−1, respectively. The hydride generated in a 170 cm reaction coil was transported to the detector with an Ar flow of 400 ml min−1. The recovery values of added concentrations, from 0.1 to 0.9 ng ml−1, o…
Determination of arsenite, arsenate, monomethylarsonic acid and dimethylarsinic acid in cereals by hydride generation atomic fluorescence spectrometry
2007
Abstract A fast, sensitive and simple non-chromatographic analytical method was developed for the speciation analysis of toxic arsenic species in cereal samples, namely rice and wheat semolina. An ultrasound-assisted extraction of the toxic arsenic species was performed with 1 mol L− 1 H3PO4 and 0.1% (m/v) Triton XT-114. After extraction, As(III), As(V), dimethylarsinic acid (DMA) and monomethylarsonic acid (MMA) concentrations were determined by hydride generation atomic fluorescence spectrometry using a series of proportional equations corresponding to four different experimental reduction conditions. The detection limits of the method were 1.3, 0.9, 1.5 and 0.6 ng g− 1 for As(III), As(V)…