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Query: KEGG:D04839 (Florisil)
 775 document(s) hit in 31,850,051 MEDLINE articles (0.00 seconds)

Method 8080, as published in the Second Edition of "Test Methods for Evaluating Solid Waste," EPA Manual SW-846, has been evaluated in a single-laboratory study. The Florisil procedure recommended in Method 8080 for sample cleanup does not separate organochlorine pesticides (OCPs) from the polychlorinated biphenyls (PCBs). Consequently, gas chromatographic analysis of OCPs on the packed column recommended in the method may result in false identifications or in no identifications at all when PCBs are present. Therefore, silica gel was substituted for Florisil, a capillary column was substituted for the packed column, and a sulfur cleanup procedure was incorporated in the method. The revised method was evaluated with samples spiked at 3 concentrations. Precision and accuracy indicate that the revised method can be reliably applied to the determination of OCPs and PCBs in liquid and solid matrixes. Detection limits for liquid matrixes range from 0.02 to 0.09 micrograms/L for OCPs and from 0.5 to 0.9 micrograms/L for PCBs. Detection limits for solid matrixes range from 1 to 6 micrograms/kg for OCPs and from 60 to 70 micrograms/kg for PCBs.
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PMID:Single-laboratory evaluation of EPA method 8080 for determination of chlorinated pesticides and polychlorinated biphenyls in hazardous wastes. 283 50

A method, previously used for determination of 2,3,7,8-substituted polychlorinated dibenzo-p-dioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs), has been modified for quantitative analysis of "dioxin-like" polychlorobiphenyls (PCBs) in environmental samples from the steel industry. The existing sample clean-up procedure, involving liquid chromatography on multi-layered silica and Florisil columns, has been extended to include a third chromatography stage on a basic alumina stationary phase. The additional clean-up stage is required for PCB analysis in order to eliminate interferences from relatively large concentrations of saturated cyclic and aliphatic hydrocarbons. Samples were analysed for WHO-12 congeners using high resolution gas chromatography/high resolution mass spectrometry (HRGC/HRMS) and standard solutions of the method US EPA 1668A. Replicate analysis of method blanks revealed background contamination for PCBs 118, 105 and 77, which are generally abundant in ambient air. These contaminants were taken into account using a subtraction method. The entire procedure was validated by replicate analysis (N = 3) of a certified reference sediment. The RSD for each WHO-12 congener was below 15%, 13C12-labelled PCB internal standard recoveries were in the range 70-95%. A waste dust sample collected in the electrostatic precipitator of a UK sinter plant was analysed for determination of PCDD/Fs and WHO-12 PCBs and exhibited a PCDD/F I-TEQ of 148.5 +/- 21.2 ngkg(-1) and a WHO-TEQ of 7.2 +/- 1.5 ngkg(-1). WHO-12 congeners contributed only 4.6% to the overall TEQ and PCB 126 was the major congener contributing to the WHO-TEQ (96%). The contribution to the overall TEQ of the waste dust sample was mainly attributed to PCDF followed by PCDD, which accounted for 86.6% and 8.7% to the overall TEQ, respectively.
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PMID:Development and validation of a method for analysis of "dioxin-like" PCBs in environmental samples from the steel industry. 1455 54

An enzyme-linked immunosorbent assay (ELISA) method was developed to quantitatively measure 2,4-dichlorophenoxyacetic acid (2,4-D) in human urine. Samples were diluted (1:5) with phosphate-buffered saline containing 0.05% Tween and 0.02% sodium azide, with analysis by a 96-microwell plate immunoassay format. No clean up was required as dilution step minimized sample interferences. Fifty urine samples were received without identifiers from a subset of pesticide applicators and their spouses in an EPA pesticide exposure study (PES) and analyzed by the ELISA method and a conventional gas chromatography/mass spectrometry (GC/MS) procedure. For the GC/MS analysis, urine samples were extracted with acidic dichloromethane (DCM); methylated by diazomethane and fractionated by a Florisil solid phase extraction (SPE) column prior to GC/MS detection. The percent relative standard deviation (%R.S.D.) of the 96-microwell plate triplicate assays ranged from 1.2 to 22% for the urine samples. Day-to-day variation of the assay results was within +/-20%. Quantitative recoveries (>70%) of 2,4-D were obtained for the spiked urine samples by the ELISA method. Quantitative recoveries (>80%) of 2,4-D were also obtained for these samples by the GC/MS procedure. The overall method precision of these samples was within +/-20% for both the ELISA and GC/MS methods. The estimated quantification limit for 2,4-D in urine was 30ng/mL by ELISA and 0.2ng/mL by GC/MS. A higher quantification limit for the ELISA method is partly due to the requirement of a 1:5 dilution to remove the urine sample matrix effect. The GC/MS method can accommodate a 10:1 concentration factor (10mL of urine converted into 1mL organic solvent for analysis) but requires extraction, methylation and clean up on a solid phase column. The immunoassay and GC/MS data were highly correlated, with a correlation coefficient of 0.94 and a slope of 1.00. Favorable results between the two methods were achieved despite the vast differences in sample preparation. Results indicated that the ELISA method could be used as a high throughput, quantitative monitoring tool for human urine samples to identify individuals with exposure to 2,4-D above the typical background levels.
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PMID:Development and evaluation of an enzyme-linked immunosorbent assay (ELISA) method for the measurement of 2,4-dichlorophenoxyacetic acid in human urine. 1897 Feb 21

Seventeen polychlorinated dibenzo-p-dioxins and polychlorinated dibenzofurans (PCDD/PCDFs) of the highest priority as well as twelve dioxin-like polychlorinated biphenyls (dl-PCBs) were analyzed in the muscle tissues of the following freshwater fish species sampled from eleven Latvian freshwater lakes: perch (Perca flavescens), carp (Cyprinus carpio), eel (Anguilla rostrata), bream (Abramis brama), chub (Leuciscus cephalus), pike (Esox lucius), sheatfish (Silurus glanis) and roach (Rutilus). To analyze the selected persistent organic pollutants in fish matrices, an optimization of EPA-1613 and EPA-1668A clean-up procedures was carried out, followed by validation of the analytical procedure according to Commission Regulation (EC) No 1883/2006. The adopted analytical procedure was in compliance with requirements of the more recent Commission Regulation (EU) No 252/2012. Modifications of carbon column chromatography clean-up and separation steps were used for treatment of the fish samples. Other clean-up procedure stages were performed according to the methods EPA-1613 and EPA-1668A and involved gel permeation chromatography (GPC), as well as manual acidic silica and Florisil column chromatography for purification and fractionation of the samples. An isotope dilution method was used for the qualitative and quantitative determination of individual congeners. Analytes of interest were separated and detected using gas chromatography - high resolution mass spectrometry. The concentration of PCDD/PCDFs and dl-PCBs in freshwater fish and eel samples ranged from 0.05 to 8.0 pg WHO(1998)-PCDD/PCDF-PCB-TEQ g(-1) fresh weight. These levels are below the EU maximum permissible limits although calculation of the content of these compounds relative to the weight of fat shows contamination levels similar to those found in Baltic herring and sprats, that are known to be highly contaminated. A difference in congener pattern between the Baltic Sea fish and freshwater fish was detected with lower contribution of 2,3,4,7,8-PeCDF to the contamination of inland water fish.
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PMID:Content of polychlorinated dibenzo-p-dioxins, dibenzofurans and dioxin-like polychlorinated biphenyls in fish from Latvian lakes. 2333 27