Showing papers on "Detection limit published in 2004"

Determination of bisphenol A in human breast milk by HPLC with column-switching and fluorescence detection.

Abstract: A highly sensitive HPLC method was developed for the determination of xenoestrogenic compound, bisphenol A (BPA) in human breast milk samples. After a two-step liquid-liquid extraction, BPA was derivatized with fluorescent labeling reagent, 4-(4,5-diphenyl-1H-imidazol-2-yl)benzoyl chloride (DIB-Cl). The excess fluorescent reagent could be removed effectively using a column-switching system. The separation of DIB-BPA from endogenous materials in milk was carried out on two C(18) columns and fluorescence intensity was monitored at 475 nm with the excitation of 350 nm. A good linearity (r = 0.994) was observed of BPA in the concentration range of 0.2-5.0 ng mL(-1) in breast milk, and the detection limit was 0.11 ng mL(-1) at a signal-to-noise ratio of 3. Intra- and inter-day precision (RSD, %) were less than 8.7 and 10.4, respectively. Twenty-three breast milk samples of healthy lactating women were analyzed for the BPA concentration; the mean value was 0.61 +/- 0.20 ng mL(-1), with no correlation to the lipid content of milk samples.

Sensitive determination of acidic drugs and triclosan in surface and wastewater by ion-pair reverse-phase liquid chromatography/tandem mass spectrometry.

Abstract: A new method is presented for the determination of 12 acidic pharmaceuticals (non-steroidal antiinflammatory drugs and bezafibrate), including two metabolites from aqueous samples, together with triclosan as a personal care product. Ion-pair liquid chromatography (IP-LC) with electrospray ionisation tandem mass spectrometry (ESI-MS) in the negative ion mode was employed. The ion-pairing agent (tri-n-butylamine) increased the signal intensity for all acidic analytes and detection limits of 6-200 ng/L were obtained by multiple reaction monitoring. This allows analysis of waste-water samples by direct injection into the LC/MS system without the need for a preceding enrichment step. When combined with a solid-phase extraction (SPE) step, limits of quantification between 0.15 and 11 ng/L were obtained from 100-mL sample volumes, which is adequate for most applications. The occurrence of matrix effects was studied and standard addition was required for reliable quantification after SPE from wastewater. The method was finally applied to surface and wastewaters, with analyte concentrations ranging from below the detection limit up to 5.5 μg/L. Copyright © 2004 John Wiley & Sons, Ltd.

LIBS limit of detection and plasma parameters of some elements in two different metallic matrices

Abstract: In the present work a detailed study has been performed on the effect of the matrix on the limit of detection (LOD) and the plasma parameters of the laser induced breakdown spectroscopy (LIBS) technique The LOD of magnesium, silicon, manganese and copper as minor elements was evaluated in aluminium standard sample alloys compared to the values of the LOD of the same elements in standard steel alloys The effect of changing the matrix on the laser induced plasma plume parameters, namely the plasma temperature Te and the electron density Ne, has been also studied Calibrations were achieved for the four elements with linear regression coefficients between 98–99% on average According to the obtained results Mn and Cu have the lowest LOD in the steel alloy matrix, while Mg has much lower LOD in the aluminium alloy matrix These results may be interpreted in view of the compatibility of the physical properties of the elements existing in the same matrix Approximately similar electronic structure and values of melting point, density, atomic weight, etc, may facilitate better conditions for energy transfer within the matrix From the application view point, it is possible for LIBS in the on-line industrial process control to follow up only a single element (that with the lowest LOD in such matrix) as a marker for the correct alloying in metals and mixing in pharmaceuticals

Determination of 5-fluorouracil in hospital effluents.

Abstract: Cytostatic anticancer drugs are an increasingly important issue in the environmental debate, mainly due to the lack of knowledge about the fate of these toxic substances. Over the last decades, 5-fluorouracil (5-FU) has been one of the most frequently used antineoplastic agents and may, therefore, be regarded as one of the pilot substances for environmental contamination. As a prerequisite for these investigations, a method for the determination of 5-FU in hospital effluents has been developed. Waste water samples were enriched by solid-phase extraction on ENV+ columns (concentration factor 500) and analysed by capillary electrophoresis using a buffer containing 80% 160 mM sodium borate buffer (pH 9.5) and 20% acetonitrile (v/v). This method is applicable within the range 5–500 μg 5-FU L−1. The standard curve (correlation coefficient >0.99) was linear with recovery rates from 80 to 96% and an accuracy from 9.0 to 20% (intra-assay standard deviation 0.7–8.9%; inter-assay standard deviation 2.2–9.5%). Based on the consumption of 5-FU in oncologic departments and the detection limit of 1.7 μg L−1, this method covers the range necessary to evaluate 5-FU in hospital effluents. The applicability of the method was proven by chemical analysis of real hospital waste water samples. Obtained over a time period of 1 month (range 20–122 μg 5-FU L−1), the results were similar to those calculated by an input–output model. The presented method provides an analytical tool necessary to face the monitoring of environmental contamination problems.

A polypyrrole-based solid-contact Pb(2+)-selective PVC-membrane electrode with a nanomolar detection limit

Abstract: Ion-selective electrodes (ISE) based on conventional plasticized PVC membranes with solid inner contact (SC) have so far had unsatisfactory lower detection limits. Here it is shown that electropolymerization of pyrrole in the presence of potassium hexacyanoferrate(II)/(III) on Pt results in adequate inner contact for SC-ISE. The nanomolar lower detection limit achieved with the Pb2+-selective PVC membranes investigated is comparable with values obtained with optimized internal solutions of liquid-contact ISE.

Electro-oxidation and amperometric detection of chlorinated phenols at boron-doped diamond electrodes: a comparison of microcrystalline and nanocrystalline thin films.

Abstract: We report on the electro-oxidation and amperometric detection of phenol and chlorinated phenols, the latter coupled with flow injection analysis (FIA) and high performance liquid chromatography (HPLC), using boron-doped microcrystalline and nanocrystalline diamond thin-film electrodes. The low background current, good response without extensive pretreatment, and low susceptibility to fouling are properties that make diamond an attractive new electrode for monitoring this class of pollutants. Cyclic voltammetric studies were performed to evaluate the redox response of phenol, 2-chlorophenol, 3-chlorophenol, 4-chlorophenol, and pentachlorophenol (PCP) in phosphate buffer, pH 3.5, as a function of the potential scan rate and cycle number. The diamond electrode performance for the amperometric detection of these contaminants in FIA-EC and HPLC-EC was evaluated in terms of the linear dynamic range, limit of quantitation, sensitivity, response precision, and response stability. Both diamond types yielded low ma...