Determination Of Pentachlorophenol Research Articles

Determination of pentachlorophenol in environmental samples of the S. Euboic Gulf, Greece.

Laboratory of Pesticides Toxicology, Benaki Phytopathological Institute, 8 Stephanou Delta Street, GR 145 61 Kifissia, Athens, Greece Laboratory of Pesticides Residues, Benaki Phytopathological Institute, 8 Stephanou Delta Street, GR 145 61 Kifissia, Athens, Greece Laboratory of Chemical Analysis of Pesticides, Benaki Phytopathological Institute, 8 Stephanou Delta Street, GR 145 61 Kifissia, Athens, Greece

Determination of Pentachlorophenol (PCP) in Samples of the Environmental Specimen Bank Using Isotope Dilution

Within the program of the Environmental Specimen Bank a quick and efficient method for determination of pentachlorophenol (PCP) in various environmental matrices has been developed. The method includes alkaline hydrolysis of bound PCP, acidification, simultaneous steam distillation and extraction in one glass apparatus. After clean-up and derivatization with acetic anhydride the samples were analyzed by gas chromatography/mass spectrometry. Concentrations were calculated using 13C-labeled PCP as the internal standard. Validation was carried out with various environmental samples (soil, fish, conifer needles, kale). The method can be used for various biological samples without any modification. The extracts are free of matrix components (lipids, chloropyll, terpenes, etc.) and other contaminants, which results in clear chromatograms with few peaks; therefore, correct integration is facilitated. Although the recoveries of PCP are in the range of 50–90%, due to losses during the several method steps, these losses can be corrected with the 13C-labeled internal standard, resulting in high precision (1.5–2.2% standard deviation).

Determination of pentachlorophenol in certified waste waters, soil samples and industrial effluents using ELISA and liquid solid extraction followed by liquid chromatography

The Pentachlorophenol RaPID-ELISA was compared with on-line liquid solid extraction (LSE) followed by liquid chromatography (LC) for the monitoring of pentachlorophenol (PCP) in certified waste waters, a waste water sample from a pulp industry, a soil sample from Brazil and a certified reference material. The water pH (1 to 9), and two cross-reactants (2,3,5,6-tetrachlorophenol and 2,3,4,6-tetrachlorophenol) were also evaluated to know if these parameters could affect the enzyme linked immunosorbent assay (ELISA) determinations. Water samples were spiked with certified material provided by Aquacheck, containing pentachlorophenol and 2,4,6-trichlorophenol at concentration levels ranging from 1 to 10 μg 1 −1. Good correlations were found between the data obtained by ELISA and from on-line LSE-LC using PLRP-S sorbent and UV detection. A dried contaminated industrial soil used as certified reference material from the Community Bureau of Reference (BCR) of the European Commission (EC), a soil sample containing pentachlorophenol at low level (μg g −1) and a waste water sample from a pulp industry were also studied using both techniques. Moreover, the confirmation of all analytes present in the waste water was carried out by liquid chromatography-mass spectrometry (LC-MS) using atmospheric pressure interface (APCI). The presence of unknown cross-reactants in the waste water affected the ELISA determinations.

Determination of pentachlorophenol in drinking water

In this study, an in situ derivatization and extraction method for the determination of pentachlorophenol (PCP) has been applied successfully in the analysis of water samples. The PCP derivative analysis was performed by gas-liquid chromatography with electron capture detection. The limit of detection of the method is 1 mg/L and recoveries averaged 78-108% for PCP acetate at levels of 2, 10 and 20 mg/L.

Determination of pentachlorophenol in commercially prepared lyophilized human urine control samples

Commercially available reference materials consisting of lyophilized human urine are routinely utilized by clinical chemists to monitor laboratory performance for a variety of analyses. In this study commercially prepared lyophilized human urine control samples were reconstituted and analyzed for pentachlorophenol. Based on replicate analyses of two different reference materials, the levels of PCP in each were found to be representative of the levels typically present in urine samples collected from the general population of the province of Saskatchewan.

Determination of pentachlorophenol in water samples by capillary zone electrophoresis

Different alternatives are presented for the monitoring of pentachlorophenol (PCP) in water samples by capillary zone electrophoresis. Detection and quantification limits can be adjusted to the required levels by means of sample stacking techniques (with or without sample matrix removal) which, together with the use of extended light path capillaries, allow the determination of PCP in the ppt range required by environmental and toxicological international regulations.

Determination of Pentachlorophenol in Water and Soil by a Magnetic Particle-Based Enzyme Immunoassay

A competitive enzyme immunoassay using specific pentachlorophenol (PCP) antiserum covalently coupled to a magnetic particle solid phase has been developed for the detection of PCP in water and soil. The immunoassay allows the quantification of PCP from 100 ppt(parts per trillion, ng/L) in water and 100 ppb (parts per billion, mg/L) in soil. Spike recovery from water samples with no sample pretreatment and from various soil types following a simple extraction technique averaged 105% and 94%, respectively. The method compares favorably with GC/MS and HPLC measurements in water (r=0.980) and soil (r=0.996) samples.

Determination of Pentachlorophenol and Cymiazole in Water and Honey by C-18 Solid Phase Extraction and Quantitative HPTLC

Abstract Pentachlorophenol and cymiazole were extracted from water and honey using C-18 solid phase extraction, column eluates were chromatographed on a high performance preadsorbent silica gel plate containing a fluorescent phosphor, and the pesticides were quantified by densitometric scanning of fluorescence quenching. Recoveries from water at concentrations of 0.25–5 ppm ranged from 97.7 to 100% for PCP and 89.5–94.9 for cymiazole. Recoveries from honey at 10 and 50 ppm ranged from 94.0–96.1% for PCP and 91.9–93.7 for cymiazole.

Determination of Pentachlorophenol and its Hydrocarbon Solvent in Wood, Soil, and Water by Gas Chromatography and FT-IR Spectroscopy in a Single-Sample Treatment

This analytical method offers a new way of measuring pentachlorophenol (PCP) in soil, wood, and water samples by gas chromatography and its hydrocarbon solvent by FT-IR spectroscopy. The distinctive feature of this method is that both the PCP and the oil are extracted from a single 1-g sample. They are first extracted from the wood or soil samples with a 1:1 mixture of Freon 113 and methanol using ultrasonication. An aliquot of the resulting organic phase is then added to an aqueous phase buffered at pH 9.2 with Na 2 HPO 4 . The oil remaining in the organic phase is analyzed by FT-IR, whereas the PCP in the aqueous phase is acetylated by reaction with acetic anhydride, back-extracted in Freon 113, and injected into the gas chromatograph. Low-PCP-content water samples ( 5 μg/L) are buffered and treated as the buffered aqueous phase. Extraction recoveries for the different matrices range from 94 to 115%. The absolute detection limits (3) for PCP and the hydrocarbon solvent are respectively 28 ng and 0.1 mg for a 1-g solid sample or a 100-mL volume of water sample. The PCP content of wood samples was compared with that obtained by neutron activation analysis and correlated with a 0.97 coefficient. The precision of the analitycal method is better than 10% for both analytes. This analytical approach was successfully applied to the radial characterization of freshly treated poles for their PCP and oil contents

Determination of Pentachlorophenol by Exhaustive Methylation and Capillary Gas Chromatography in Sewage Sludge, Contaminated Water and Suspended Particulates

Abstract A method for the determination of pentachlorophenol (PCP) in large volumes of sea water and suspended particulate matter is described. PCP is methylated using methyl iodide in the presence of tetra-butylammonium hydroxide (TBA). The methyl derivative, pentachloroanisole, is quantified by capillary gas chromatography using electron-capture detection. Recovery and the coefficient of variation of the analytical method are found to be: 78% and 4.6% respectively, (n = 17). The PCP is extracted from the sea water by liquid-liquid partition with pentane and sulphuric acid, and by soxhlet extraction with hexane:acetone, 40:60, plus sulphuric acid from the particulate matter. These extraction procedures are also effective for a wide range of other organic contaminants including sterols, chlorinated pesticides and PCBs. The sample clean-up and PCP separation are achieved by liquid-liquid extraction with alkali to isolate the acidic compounds. The PCP is back-extracted into organic solvent after acidifying ...

Determination of Pentachlorophenol in Animal Tissues: A Canadian Perspective

Analytical methods for pentachlorophenol (PCP) residues in edible animal tissue have been reviewed, with particular reference to gas chromatographic methods of analysis. Results of analyses demonstrate that significant residues of PCP can persist for several weeks in animals exposed to contaminated bedding. National surveys in Canada have found that the incidence of PCP residues in pork in excess of 0.1 ppm was reduced from 32% of survey samples in 1981-1982 to 6.6% of samples tested in 1987-1988. An interlaboratory sample exchange among Canadian laboratories demonstrated that the PCP analytical method currently used by Agriculture Canada could be successfully transferred to other laboratories. An exchange of samples between regulatory laboratories of Agriculture Canada and the Food Safety and Inspection Service of the U.S. Department of Agriculture (USDA) demonstrated equivalency of results for the 2 methods currently used in the respective laboratories, with relative standard deviations for analytical results ranging from 4.4 to 22.2%.

Simultaneous determination of pentachlorophenol and neutral organochlorine compounds in human milk

A method was developed for determining pentachlorophenol (PCP) in human milk; this method allows for analysing PCP simultaneously with neutral organochlorine compounds. The organochlorine residues determined in milk samples of 5 women were: neutral compounds such as α-, β-, γ-hexachlorocyclohexane (HCH), hexachlorobenzene (HCB), p,p'-dichlorodiphenyltrichloroethane (DDT), p,p'-dichlorodiphenyldichloroethylene (DDE), polychlorinated biphenyls (PCB's) and the acidic pentachlorophenol (PCP). The procedure is a modification of Steinwandter's method and consists of a simultaneous extraction and clean-up using silica gel leading to two different fractions, the first containing the neutral organochlorine compounds, the second PCP. Compounds in both fractions were quantified by gas chromatography (ECD); compounds in the neutral fraction directly, PCP after pyrolytic ethylation by triethylsulfonium hydroxide to pentachlorophenylethyl ether. Levels of PCP in human milk of 5 different women ranged from 0.21 to 8.5 μg/l (median: 1.47 μg/l, n=33).

Determination of pentachlorophenol by high performance thin layer chromatography

Determination of pentachlorophenol by high performance thin layer chromatography

Validation Study of Gas Chromatographic Determination of Pentachlorophenol in Animal Liver

A validation study was conducted of a gas chromatographic procedure for the determination of pentachlorophenol (PCP) in chicken, pork, and beef liver. Five analysts representing 5 laboratories analyzed randomly numbered blind duplicates at 3 fortified tissue concentrations and one incurred tissue on 2 consecutive days. The PCP concentrations ranged from approximately 40 to 400 parts per billion (ppb). All data were reported to 3 significant figures in ppb. The coefficients of variation for repeatability were between 2.8 and 8.5%, except for the beef liver, at a mean value of 80 ppb PCP, where the CV was 11.3%. The CVs for reproducibility were in the range of 9.7-16.5% with little significant difference by species. The CV asymptotically approached 10% as the PCP level increased.

Determination of pentachlorophenol in rabbit and human liver using liquid chromatography and gas chromatography with electron-capture detection

A method has been developed for the determination of ppb levels of pentachlorophenol (PCP) in liver by column liquid chromatography with on-line electron-capture detection (LC-ECD). The technique is compared with gas chromatography-ECD (GC-ECD) for the analysis of rabbit and human livers. Good results were generally obtained for LC-ECD down to the low-ppb range; however, in some cases problems were observed when the sample is not dissolved in the LC eluent. LC-ECD can adequately be used as a confirmation method for GC-ECD.

Analysis of Phenols by Chemical Derivatization. V. Determination of Pentachlorophenol and 19 Other Chlorinated Phenols in Sediments

Abstract A method for quantitative and isomer-specific analysis for pentachlorophenol and 19 other chlorophenols in sediment was developed. After acidification to pH <1, sediment samples were Soxhlet-extracted with acetone-hexane (59 + 41, v/v) for 20 h. Phenols in the organic extract were back-extracted into 2% KHCO, and were then acetylated with acetic anhydride and extracted with petroleum ether. After evaporation to a small volume, the acetates were cleaned up on a 5% deactivated silica gel column. Extracts were then analyzed on a 12 m OV-1 column interfaced to an electron-capture detector and on a 30 m SPB-5 column interfaced to a mass selective detector. The procedure has been validated with sediment samples fortified at 100, 10, and 1 ng/g levels of chlorophenols. Recoveries of dichloro- and the higher chlorophenols were generally between 80 and 95% at all 3 levels of fortification, whereas recoveries of monochlorophenols were between 65 and 85%. The 2 chloromethylphenols were less than 50% recovered, and recovery of phenol itself was erratic by this procedure. Using a 50 g sample size, the estimated detection limit was ca 0.2 ng/g.

Determination of pentachlorophenol (PCP) in human serum and urine using triethylsulfonium hydroxide for pyrolytic ethylation

A method to analyze pentachlorophenol (PCP) in human serum and urine is described. Sample preparation involves extraction of PCP with toluene after acidification of serum (0.5 ml) or acidic hydrolysis of urine (1 ml). The toluene extracts are then reextracted by an aqueous-methanolic solution of triethylsulfonium hydroxide (TESH). This phase is injected into the gas chromatograph where a pyrolytic ethylation of acidic compounds like PCP occurs. Using capillary columns for chromatography and EC detection the detection limit is 2 μg/l for urine and 3 μg/l for serum. The accuracy of the method was ensured by gas chromatography-mass spectrometry. Serum and urine concentrations of persons not exposed to PCP as well as of persons, that used wood preserving agents some years ago, are reported.

Gas Chromatographic Determination of Pentachlorophenol in Gelatin: Collaborative Study

Eleven collaborators participated in this study of a gas chromatographic method for the determination of pentachlorophenol (PCP) in gelatin. Following acid hydrolysis of a 2 g sample, PCP is extracted with hexane and partitioned into KOH solution. After reacidification, PCP is again extracted with hexane for determination by electron capture gas chromatography on a 1% SP-1240DA column. Three duplicate practice samples (0.0, 0.5, and 1.5 ppm) and 5 blind duplicate collaborative samples (0.0, 0.02, 0.1, 0.5, and 2.0 ppm) were analyzed by each collaborator. Mean recoveries of PCP in the collaborative samples ranged from 88% at the 0.02 ppm fortification level to 102% at the 0.1 ppm level; the overall mean recovery was 96%. Interlaboratory coefficients of variation ranged from 16.4% for the 0.1 ppm fortification level to 22.9% for the 0.5 ppm level; the overall interlaboratory coefficient of variation was 19.5%. The method has been adopted official first action.

Capillary Gas Chromatographic Determination of Pentachlorophenol Residues in Tallow Following Automated Gel Permeation Cleanup

Abstract A gas chromatographic method for the determination of pentachlorophenol (PCP) in tallow is described. Samples are melted and mixed with the solvent used for automated gel permeation chromatographic (GPC) cleanup. The methyl ether derivative of PCP is prepared by treating the appropriate GPC fraction with an ethereal solution of diazomethane. The extract is further cleaned up on Florisil, and the PCP methyl ether is easily identified and quantified by capillary column gas chromatography (GC) with electron capture detector. The detection limit was 0.001 ppm in tallow. Recoveries varied from 80 to 107% over the fortification range of 0.005–0.05 ppm. Capillary GC-high resolution mass spectrometry is used to confirm PCP methyl ether in the sample extract.

Gas Chromatographic Determination of Pentachlorophenol in Gelatin

A method is described for the determination of pentachlorophenol (PCP) in gelatin. The method employs acid and heat to hydrolyze the gelatin matrix, a base partition and wash for separation and cleanup, and a reacidification and extraction with hexane for direct determination of PCP, without preparation of a derivative, using gas chromatography (GC) with a 1% SP- 124ODA liquid phase and a 63Ni electron capture detector. Recoveries averaged 106% for fortifications between 0.02 and 1.0 ppm. The limit of quantitation is 20 ppb. The limit of detection is 4-6 ppb. The method, which has undergone a successful intralaboratory trial, is simple and rapid, and requires only general laboratory reagents and equipment. GC of the acetate derivative of PCP is used for confirmation of identity.