Search results for "Detection limit"
showing 10 items of 810 documents
Optimization of large-volume injection for the determination of polychlorinated biphenyls in children's fast-food menus by low-resolution mass spectr…
2008
International audience; This study includes the determination of five indicator polychlorinated biphenyls (PCBs) (52, 101, 153, 138, and 180), six non-ortho PCBs (35, 80, 81, 77, 126, and 169), and two mono-ortho PCBs (28 and 118) in fast food for children. A freeze-dried sample of 10 g is extracted by using pressurized n-hexane in two 5 min cycles at 120 degrees C and 100 mbar. Fatty extracts were cleaned up by means of acetonitrile/n-hexane partitioning and gel-permeation chromatography. The fractionation of non-ortho, mono-ortho, and indicator PCBs was made on graphitized carbon solid-phase extraction cartridges by using n-hexane, n-hexane/toluene (99:1, v/v), and toluene as elution solv…
Determination of ultratrace bismuth in milk samples by atomic fluorescence spectrometry.
2003
Abstract A sensitive procedure was developed for determination of bismuth (Bi) in milk samples by hydride generation atomic fluorescence spectrometry (HG–AFS) after microwave-assisted sample digestion with HNO3 and H2O2. The method provides a sensitivity of 1832 fluorescence units (ng/mL) with a detection limit of 0.01 ng/mL, which corresponds to 20 pg absolute limit of detection, equivalent to 0.50 ng/g in the original sample. Application of the methodology to cow milk samples from the Spanish market showed the presence of Bi at a concentration of 11.8–28.8 ng/g, which compared well with data obtained after dry ashing of samples and with data obtained by inductively coupled plasma–mass spe…
Use of polarography as a quality-control method for determining diacetyl in citrus and vegetable juices, yoghurt and butter
2002
The determination of diacetyl permits the detection of microbial growth in the processing of citrus fruit before the appearance of other organoleptic, chemical or microbiological changes. It also makes it possible to detect a break in the cold chain during distribution and sale. The study proposed a polarographic method for the determination of diacetyl that allowed routine analysis with the aim of detecting possible contamination in the citrus juice manufacturing chain (orange and orange-carrot). The analytical performance of the method in terms of a linearity from 0 to 960 microg ml(-1), a recovery of 97 to 98%, a precision of 3.2 to 4.8%, and a sensitivity of 0.2 ng ml(-1) for juices ind…
Quality control Fourier transform infrared determination of diazepam in pharmaceuticals
2007
A quality control procedure has been developed for the determination of diazepam in pharmaceuticals using Fourier transform infrared (FTIR) spectroscopy. The method involves the off-line extraction of diazepam with chloroform by sonication and direct determination in the extracts through peak area measurement in the interval between 1672 and 1682 cm(-1) using a baseline correction defined between 1850 and 1524 cm(-1). For standardization it was used an external calibration line established from standard solutions of diazepam in chloroform. The method provides a limit of detection of 0.04 mg per tablet (n=5), a relative standard deviation (R.S.D.) of 0.5% for 5 independent measurements of a …
Absence Ochratoxin A in soy sauce
2004
A method is described for the determination of ochratoxin A (OTA) in soy sauce using phosphate-buffered saline (PBS) extraction, an immunoaffinity clean-up, a liquid chromatographic determination with fluorescence detection (LC-FD) and confirmation with LC-FD after methylation of OTA. Recoveries of OTA spiked to soy sauce samples at 0.25 ng/ml level were 90% with relative standard deviations of 4%. The limit of detection was 0.01 ng/ml for OTA using the proposed method. Furthermore, the proposed method was applied to 60 soy sauce samples from China and Japan and none of them were found to contain OTA.
Quality control of fruit juices by using organic acids determined by capillary zone electrophoresis with poly(vinyl alcohol)-coated bubble cell capil…
2015
An enhanced method for the determination of organic acids in several fruit juices by capillary zone electrophoresis (CZE) with direct UV-Vis detection has been developed in this work. First, a study with simulated real juice samples was done to find the best separation conditions. Next, several commercial fruit juices were analyzed, and the organic acid contents were quantified in less than 12 min using a poly(vinyl alcohol)-coated fused-silica 'bubble cell' capillary. The present method is reliable, fast and provides detection limits comprised between 0.1 and 2.5 μg mL(-1). Moreover, different chemometric techniques, based on CZE data, were examined. Linear discriminant analysis allowed th…
Iodine determination in food samples using inductively coupled plasma isotope dilution mass spectrometry.
1998
Two different sample treatment methods are used in connection with inductively coupled plasma isotope dilution mass spectrometry for accurate and precise determinations of iodine traces in food samples. 129I-enriched iodate is applied as a spike compound for the isotope dilution step. Extraction of iodine by tetramethylammonium hydroxide (TMAH) solution at high temperatures in a closed vessel is one of the sample treatment methods. The other one is a complete decomposition of the sample with a mixture of perchloric acid and nitric acid using microwave assistance. By analyzing different certified reference materials (three milk powders with different iodine levels, BCR CRM 63, 150, and 151; …
Rugged Large Volume Injection for Sensitive Capillary LC-MS Environmental Monitoring
2017
A rugged and high throughput capillary column (cLC) LC-MS switching platform using large volume injection and on-line automatic filtration and filter back-flush (AFFL) solid phase extraction (SPE) for analysis of environmental water samples with minimal sample preparation is presented. Although narrow columns and on-line sample preparation are used in the platform, high ruggedness is achieved e.g. injection of 100 non-filtrated water samples would did not result in a pressure rise/clogging of the SPE/capillary columns (inner diameter 300 µm). In addition, satisfactory retention time stability and chromatographic resolution were also features of the system. The potential of the platform for …
Determination of liposoluble vitamins in cooked meals, milk and milk products by liquid chromatography
2002
A method for the simultaneous determination of liposoluble vitamins in cooked meals was established. Saponification was performed with 50% (w/v) KOH at 80 degrees C, and ascorbic acid was added as antioxidant. The subsequent extraction was carried out with diethyl ether. This was followed by a liquid chromatographic separation on a reversed-phase C18 column with methanol-water (94:6, v/v as the mobile phase. Retinyl acetate was used as the internal standard. The analytical parameters linearity, detection limit (0.19 and 8.33 microg/100 g for retinol and alpha-tocopherol, respectively), precision of the method (RSD=5.24 and 6.99% for retinol and alpha-tocopherol, respectively) and recovery a…
On-line in-tube solid phase microextraction coupled to capillary liquid chromatography-diode array detection for the analysis of caffeine and its met…
2019
Abstract In-tube solid phase microextraction (IT-SPME) coupled on-line to capillary liquid chromatography with diode array detection provides a simple and fast analytical methodology for the simultaneous quantitation of caffeine and its three primary metabolites (theobromine, paraxanthine and theophylline) in micro samples of serum, saliva and urine matrices. The sample amount required for one analysis was only 2.5 μL of saliva, 6.25 μL of serum or 40 μL of urine, a requirement for its implementation in a hospital laboratory for preterm newborns, where sample availability is a major problem. In standard conditions, 25 μL of diluted saliva or serum (or 100 μL of urine) were processed by IT-S…