Determination Of Pentachlorophenol Research Articles

Determination of Pentachlorophenol in Seafood Samples from Zhejiang Province Using Pass-Through SPE-UPLC-MS/MS: Occurrence and Human Dietary Exposure Risk.

Pentachlorophenol (PCP) has attracted wide attention due to its high toxicity, persistence, and bioaccumulation. In this study, a sensitive UPLC-MS/MS method for the determination of PCP in seafood samples was developed and validated. The samples were ultrasonic extracted with acetonitrile containing 1% acetic acid-acetonitrile and followed by using a pass-through solid-phase extraction (SPE) cleanup on Captiva EMR-Lipid cartridges. The linearity of this method ranged from 1 to 1000 μg/L, with regression coefficients of >0.99. The detection limit and quantitation limit were 0.5 μg/kg and 1.0 μg/kg, respectively. The recoveries in different types of seafood samples ranged from 86.4% to 102.5%, and the intra-day and inter-day relative standard deviations (RSDs) were 3.7% to 11.2% and 2.9% to 12.1%, respectively (n = 6). Finally, the method has been successfully utilized for the screening of PCP in 760 seafood samples from Zhejiang Province. PCP was detected in 5.8% of all seafood samples, with the largest portion of detections found in shellfish, accounting for approximately 60% of the total. The average concentrations detected ranged from 1.08 to 21.49 μg/kg. The non-carcinogenic risk indices for adults and children who consume PCP ranged from 10-4 to 10-3 magnitudes. All of these indices stayed significantly below 1, implying that the health risk from PCP in marine organisms to humans is minimal.

Determination of Pentachlorophenol in Environmental Samples by Spectrophotometry

Pentachlorophenol (PCP) (2,3,4,5,6- pentachlorophenol) is an organochlorine compound used as a pesticide and a disinfectant. PCP is used as a herbicide, insecticide, fungicide and disinfectant. Some applications include agricultural seeds (for nonfood uses), leather, masonry, wood preservation, cooling tower water, rope, and paper mills. Determination of Pentachlorophenol was based on the reaction of PCP with concentrated nitric acid followed by potassium iodide for the liberation of iodine. Liberated iodine reacted with leuco malachite green for the formation of green colour dye which was measured at 610 nm against a reagent blank. Parameters affecting the reaction were studied. The interfering effect of various species was also investigated and the methods were applied on some vegetables and fruit samples.

Determination of pentachlorophenol by anodic electrochemiluminescence of Ru(bpy)32+ based on nitrogen-doped graphene quantum dots as co-reactant

A novel ultrasensitive Ru(bpy)32+-based anodic ECL sensor using NGQDs as co-reactant was developed for PCP detection.

An environmentally friendly method for the determination of pentachlorophenol in paper packaging materials using ultrasonic-assisted micellar extraction.

Ultrasonic-assisted micellar extraction coupled with high-pressure liquid chromatography has been developed for the determination of pentachlorophenol (PCP) in paper packaging materials. A non-ionic surfactant, polyethylene glycol sorbitan monolaurate (Tween 20), was used for ultrasonic extraction and the method was applied to different paper packaging materials under optimized conditions. The recoveries for spiked samples were 83-90.1% and relative standard deviations were <5.0%. The limit of detection and the limit of quantification for PCP were 0.9 and 2.0 µg/g, respectively. Results confirmed that this relatively simple procedure proved satisfactory for the determination of PCP in paper packaging materials.

The potentiometric sensor for determination of pentachlorophenol in water

A pentachlorophenolate—a sensitive device based on an ionic associate of astraphloxine pentachlorophenol has been developed. The proposed sensor possesses satisfactory electroanalytical characteristics, which makes it possible to use it in its potentiometric determination of pentachlorophenol in water.

Determination of Pentachlorophenol in Human Urine by Homemade Ionic liquid Solid-phase Microextraction Coating

A new method for the determination of pentachlorophenol(PCP) in human urine has been developed by headspace solid-phase microextraction with gas chromatography(HS-SPME-GC).A homemade ionic liquid(IL) bonded coating solid-phase microextraction was added by the sol-gel method.The extraction conditions were optimized as the extraction temperature of 80 ℃,extraction time of 50 min by headspace,desorption time of 5 min at 300 ℃,NaCl amount of 3 g,pH of 2 and under stirring.The detection limits was 5.0 ng/L.The linear range was 0.05-100 μg/L.The relative standard deviations(RSD) was 5.9%.The recovery was 106.6%.

Electrochemical Determination of Pentachlorophenol in Water on a Multi-Wall Carbon Nanotubes-Epoxy Composite Electrode

The aim of this study was the preparation, characterization, and application of a multi-wall carbon nanotubes-epoxy composite electrode (MWCNT-EP) with 25%, wt. MWCNTs loading for the voltammetric/amperometric determination of pentachlorophenol (PCP) in aqueous solutions. The structural and morphological aspects of the MWCNT-EP composite electrode were examined by scanning electron microscopy. The electrical properties were characterized by direct-current conductivity measurements in relation with the percolation threshold. The electrochemical behavior of PCP at the MWCNT-EP composite electrode was investigated using cyclic voltammetry in 0.1 M Na2SO4 supporting electrolyte in order to establish the parameters for amperometric/voltammetric determination of PCP. The linear dependence of current vs. PCP concentrations was reached in a wide concentration range from 0.2 to 12 μM PCP using cyclic voltammetry, differential-pulsed voltammetry, square-wave voltammetry, chronoamperometry, and multiple-pulsed amperometry techniques. The best electroanalytical performances of this composite electrode were achieved using a pre-concentration/square-wave voltammetric technique and also multiple-pulsed amperometry techniques envisaging the practical applications. The ease of preparation, high sensitivity, and stability of this composite electrode should open novel avenues and applications for fabricating robust sensors for detection of many important species.

Uncertainty in the quantification of pentachlorophenol in wood processing wastewaters by SPME-GC-MS

Pentachlorophenol is a trace contaminant with toxicological effects in environment. When dealing with the analysis and quantification of trace amounts in complex matrices, procedures such as extraction/pre-concentration are often needed and chromatographic determination are often operated close to the limit of detection, which contribute to the increase of the uncertainty of the measurement. This matter is of crucial importance when the results obtained approach the legal limits and is frequently ignored in scientific work. The aim of this study was the estimation of the global uncertainty associated to the determination of pentachlorophenol (PCP) in aqueous samples, by gas chromatography with mass spectrometric detection (GC-MS), after solid-phase microextraction (SPME). It was concluded that, while in the range of 5 to 40 μg/L the uncertainty did not exceed 20%, in the vicinity of the limit of detection (0.75 μg/L) it raised up to 64%.

Dispersive liquid-liquid microextraction and liquid chromatographic determination of pentachlorophenol in water

Abstract A simple and sensitive dispersive liquid-liquid microextraction method for extraction and preconcentration of pentachlorophenol (PCP) in water samples is presented. After adjusting the sample pH to 3, extraction was performed in the presence of 1% W/V sodium chloride by injecting 1 mL acetone as disperser solvent containing 15 μL tetrachloroethylene as extraction solvent. The proposed DLLME method was followed by HPLC-DAD for determination of PCP. It has good linearity (0.994) with wide linear dynamic range (0.1–1000 μg L−1) and low detection limit (0.03 μg L−1), which makes it suitable for determination of PCP in water samples.

Immunoassay Method for the Determination of Pentachlorophenol in Soil and Sediment

Immunoassay Method for the Determination of Pentachlorophenol in Soil and Sediment

Determination of pentachlorophenol in wastewater irrigated soils and incubated earthworms

The analyses of low pentachlorophenol (PCP) in soils and earthworms require a sensitive and reliable analytical method. In this paper, several derivatization methods and extraction solvents were compared systematically. The derivatization reagents included acetic anhydride, 2,3,4,5,6-pentafluorobenzyl bromide (PFBBr) and diazomethane. Hexane, acetone, hexane–acetone (1:1), dichloromethane and methanol were used as the extraction solvents. PFBBr derivatization showed the highest sensitivity. The derivatization parameters of PFBBr including the amount of PFBBr, the power and irradiation time of microwave were optimized. As a result, 200 μl of PFBBr (10%) at 150 W of microwave oven for 30 min achieved the best result. The PFBBr derivatization method had the detection limit of 0.07 μg l −1 of PCP. Extraction by a mixture of hexane and acetone (1:1) showed the best recoveries. The recommended method was used to determine the low PCP in soils irrigated by wastewater and earthworms incubated in the corresponding soils. The concentrations of PCP in soils were in the range of 1.38–179 ng g −1, while those in earthworms were 11.2–262 ng g −1. The recoveries of the surrogate standard (trichlorophenol) ranged from 81.1% to 107%, demonstrating the merit of the method.

A Simplified Method for Determination of Pentachlorophenol and Hexachlorobenzene in Soil Contaminated by Industrial Chemical Residues

A Simplified Method for Determination of Pentachlorophenol and Hexachlorobenzene in Soil Contaminated by Industrial Chemical Residues

Determination of pentachlorophenol by negative ion chemical ionization with membrane introduction mass spectrometry.

Pentachlorophenol (PCP) was used as a model compound to explore the potential of desorption chemical ionization (DCI) in the determination of polychlorinated pesticides using membrane introduction mass spectrometry (MIMS). A direct insertion membrane probe was modified so that a chemical ionization plasma could be established at the membrane surface. Using selected ion monitoring (SIM) in a tandem triple quadrupole mass spectrometer with isobutane chemical ionization (CI), the PCP detection limit under positive chemical ionization is 20 ppb whereas negative CI gives detection limits in the low ppb range. This performance is achieved without any pre-treatment or derivatization of the sample. Negative ion CI gives a signal that is linear over a concentration range of 2-1000 ppb. Comparison of data obtained with low ppb samples of 2,4,6-trichlorophenol, 2,3,4,6-tetrachlorophenol and pentachlorophenol suggests that the sensitivity of this analytical procedure increases with increase in the number of electronegative substituents in the molecule.

Development of rotating electrochemical detectors for capillary electrophoresis.

A rotating disk electrode (RDE) has been evaluated and optimized for the detection of electroactive species separated by capillary electrophoresis (CE). With catechol as a working model, the limit of detection was estimated to be 0.3 microM, i.e., approximately 2.5-fold better than that of the stationary disk electrode (0.7 microM). Separation efficiency was significantly improved as exemplified by an increase of theoretical plates from 26,000 plates/m at 0 rpm to 67,000 plates/m at 500 rpm. Of particular importance was the capability of RDE to alleviate electrode passivation and electrical interference associated with high separation potential fields. Therefore, rotation amperometry was especially useful for analytes such as phenolic compounds that tended to rapidly foul the electrode surface. The RDE/ CE system was capable of separation and determination of pentachlorophenol in contaminated soils, and the result obtained agreed well with conventional liquid chromatography, an EPA recommended procedure.

A simple method to evaluate the concentration of pentachlorophenol degraders in contaminated soils.

A new most probable number (MPN) method for the determination of pentachlorophenol (PCP) degraders in soil using the change in pH due to PCP degradation is compared with a well documented MPN method using radiolabeled PCP. The results of all MPN counts were similar within a 95% confidence limit. The results obtained in MPN per gram of dry soil using pH measurements were 1.8 (+3.1, -1.03) x10 (4) compared to 0.64 (+1.34, -0.42) x 10(4) when using production of [(14)C]CO(2).

Determination of pentachlorophenol in human urine using solid phase extraction and GC‐MS analysis with stable isotope dilution

A method for the determination of pentachlorophenol (PCP) in human urine was developed. Urine samples were fortified with 13C6‐IabeIed PCP and hydrolyzed with sulfuric acid prior to extraction. The urine samples were then passed through preconditioned solid phase extraction cartridges containing octadecylsilane adsorbent. The PCP was subsequently eluted from the cartridge with ethyl acetate and converted to pentachloroanisole prior to GC‐MS analysis. GC‐MS quantitation was performed using the technique of stable isotope dilution. Percent recoveries averaging 100, 97, and 111% were obtained for replicate urine samples fortified with approximately 2, 20, and 200 ng/mL of PCP, respectively. The method detection limit was estimated to be 0.2 ng/mL.

Determination of Pentachlorophenol and Hexachlorobenzene in Natural Waters Affected by Industrial Chemical Residues

Este trabalho teve como principal objetivo o desenvolvimento de uma metodologia para a analise simultânea de pentaclorofenol (PCP) e hexaclorobenzeno (HCB) em agua natural de subsuperficie proveniente de uma regiao afetada por residuos industriais (Sao Vicente-SP), onde a maior parte da populacao se utiliza de pocos pouco profundos para o abastecimento. A extracao liquido-liquido apresentou bons resultados quanto a recuperacao e repetibilidade do metodo. Para o nivel de fortificacao de 10 ng L-1 de PCP e HCB a recuperacao situou-se entre 81.5% e 103.0%, com um desvio padrao relativo de 2.4% a 4.1%. A determinacao dos analitos foi efetuada por GC-ECD e/ou GC-MS. Adicionalmente, o limite de quantificacao do metodo foi de 5 ng L-1 para PCP e 2 ng L-1 para HCB, valores que estao abaixo do nivel maximo permitido pelas diretrizes da Comunidade Europeia para residuos de pesticidas em agua potavel.

Determination of Pentachlorophenol and Its Oil Solvent in Wood Pole Samples by SFE and GC with Postcolumn Flow Splitting for Simultaneous Detection of the Species

An alternative approach is described for the measurement of pentachlorophenol (PCP) and its oil solvent in wood samples by supercritical fluid extraction (SFE) and gas chromatography (GC). The determination is achieved over a single chromatographic run using postcolumn flow splitting for simultaneous ECD/FID detection of the SFE extracted species. First, PCP and oil components are quantitatively extracted from a 0.3-g wood sample using 10% MeOH/CO(2) supercritical fluid at 0.65 g/mL and 120 °C. An aliquot of the SFE solution is then mixed with 10 mL of a buffered aqueous phase at pH 9.4. After PCP is acetylated by the addition of 500 μL of acetic anhydride, it is followed by its extraction with 2.00 mL of hexane along with oil. Then, 0.5 μL of supernatant organic phase is injected into the GC for a selective and simultaneous determination of the species. The method has a linear response over 3 orders of magnitude for both species with a linear regression correlation coefficient higher than 0.98 (95% confidence limit) and an absolute detection limit of 60 ng of PCP and 80 μg of oil per 0.1-g wood sample. The precision (relative standard deviation) is 4% for PCP and 1% for oil as established for a typical average concentration sample. The accuracy of the SFE GC-ECD/FID combined technique for PCP and oil was assessed by analyzing wood samples collected from newly and in-service PCP/oil-impregnated red pine poles.

Sensitive Spectrophotometric Method for Determining Pentachlorophenol in Various Environmental Samples

A new, simple, and sensitive spectrophotometric method is described for determination of pentachlorophenol, a widely used insecticide and herbicide, in various environmental samples. The method is based on the reaction of pentachlorophenol with concentrated nitric acid to form chloranil, which liberates iodine from potassium iodide. The liberated iodine then selectively oxidizes leucocrystal violet to form crystal violet, which has an absorption maximum at 592 nm. Beer's law is obeyed over the concentration range of 0.1-1.6 micrograms pentachlorophenol/25 mL (0.004-0.064 ppm). The method was applied satisfactorily to determination of pentachlorophenol in air, water, plant material, textile effluent, and biological samples.

Performance evaluation of the Quick Test�, a colorimetric field method for the determination of pentachlorophenol in soil

A novel colorimetric-based field test kit, the Quick Test®, has been developed by Envirol Inc. (North Logan, UT), for the quantitation of pentachlorophenol (PCP) in soil. The Quick Test differs from commercially available immunoassay field tests for PCP in that it is based on a photochemically induced oxidation–reduction reaction between PCP and a reagent that produces coloration proportional to concentration. Standard quality-control procedures were used to characterize the performance of the Quick Test and to test the suitability of this new method for field investigations of PCP-contaminated sites. A method detection limit of 1.5 mg/kg was achieved with a dynamic range up to 100 mg/kg, making this procedure of practical use at many PCP-contaminated sites. Accuracy and precision for the analysis of PCP in soils were comparable to laboratory standard methods that involve Soxhlet extractions and chromatographic quantitation. Because this is an oxidation–reduction reaction between halogenated molecules and the reagent, many, but not all, halogenated organic compounds will cause a response. An acid-base cleanup stop eliminates all but acidic halogenated compounds. The performance of the Quick Test in the field was compared with laboratory results. The statistical analyses performed to determine intermethod accuracy were linear regression analysis and the Wilcoxon Signed Ranks test. All data sets had r2 values greater than 0.915 and y-intercept values and the slope of the line that were not statistically different from 0 and 1, respectively, at a 90% confidence level. Data sets were not statistically different by the Wilcoxon test (95% confidence level), confirming the results from the regression analysis—that the Quick Test provided data equivalent (1:1) to the confirmatory methods. © 1998 John Wiley & Sons, Inc. Field Analyt Chem Technol 2: 29–37, 1998