Group separation of ortho -PCBs, coplanar non- ortho -PCBs and PCDDs/PCDFs using an alumina column as an one-step clean-up procedure

Loos, Robert; Vollmuth, Stefan

doi:10.1007/s002160050309

Cited by 9 publications

(4 citation statements)

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“…The synthetic PCB derivatives prepared by the above mentioned methods are frequently purified by column chromatography using silica gel as stationary phase or recrystallization from methanol, or a combination of both approaches. It is also possible to separate ortho PCBs, non- ortho PCBs and/or polychlorinated dibenzodioxins (PCDDs)/polychlorinated dibenzofurans (PCDFs) using stationary phases such as alumina, charcoal or Florisil (Athanasiadou et al 1991, Goldstein et al 1978, Loos et al 1997, Mannila 1992, Peterman et al 2006, Porter & Burke 1971, Storrhansen et al 1992). The level of activation of the respective stationary phase is critical for a successful separation (Storrhansen et al 1992).…”

Section: Resultsmentioning

confidence: 99%

Authentication of synthetic environmental contaminants and their (bio)transformation products in toxicology: polychlorinated biphenyls as an example

Holland

Feng

et al. 2018

Environ Sci Pollut Res

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Toxicological studies use "specialty chemicals" and, thus, should assess and report both identity and degree of purity (homogeneity) of the chemicals (or toxicants) under investigation to ensure that other scientists can replicate experimental results. Although detailed reporting criteria for the synthesis and characterization of organic compounds have been established by organic chemistry journals, such criteria are inconsistently applied to the chemicals used in toxicological studies. Biologically active trace impurities may lead to incorrect conclusions about the chemical entity responsible for a biological response, which in turn may confound risk assessment. Based on our experience with the synthesis of PCBs and their metabolites, we herein propose guidelines for the "authentication" of synthetic PCBs and, by extension, other organic toxicants, and provide a checklist for documenting the authentication of toxicants reported in the peer-reviewed literature. The objective is to expand guidelines proposed for different types of biomedical and preclinical studies to include a thorough authentication of specialty chemicals, such as PCBs and their derivatives, with the goal of ensuring transparent and open reporting of scientific results in toxicology and the environmental health sciences.

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Section: Resultsmentioning

confidence: 99%

Authentication of synthetic environmental contaminants and their (bio)transformation products in toxicology: polychlorinated biphenyls as an example

Holland

Feng

et al. 2018

Environ Sci Pollut Res

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“…Isotope dilution mass spectrometry (IDMS) is a more elegant method to overcome the problem of sample recovery. 16,[26][27][28][29] In this method, a 13 C-labeled isotope of the analyte is added to the sample at the beginning of the analysis, and the ratio of labeled and unlabeled compounds is determined by MS. This technique eliminates the need for recovery measurements and automatically accounts for any loss in the determination.…”

Section: Resultsmentioning

confidence: 99%

“…Although addition of a known amount of the analyte to the matrix prior to extraction followed by a subsequent analysis does not precisely measure the extraction efficiency of naturally bound analytes, this type of spiked sample analysis will determine the accuracy and precision of the subsequent analytical steps. Isotope dilution mass spectrometry (IDMS) is a more elegant method to overcome the problem of sample recovery. ,− In this method, a 13 C-labeled isotope of the analyte is added to the sample at the beginning of the analysis, and the ratio of labeled and unlabeled compounds is determined by MS. This technique eliminates the need for recovery measurements and automatically accounts for any loss in the determination.…”

Section: Resultsmentioning

confidence: 99%

Methodological Refinements in the Determination of 146 Polychlorinated Biphenyls, Including Non-Ortho- and Mono-Ortho-Substituted PCBs, and 26 Organochlorine Pesticides as Demonstrated in Heron Eggs

et al. 2003

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A method for the determination of 146 polychlorinated biphenyls (PCBs), including four non-ortho- and eight mono-ortho-substituted congeners, and 26 chlorinated pesticides is described. The method consists of ultrasonic extraction, Florisil cleanup, HPLC fractionation over porous graphitic carbon (PGC), and final determination with GC/ECD, GC/MS, or both. Two PCB congeners (PCB 30 and PCB 161) and two polybromobiphenyls (2,4',5-tribromobiphenyl and 3,3',4,4'-tetrabromobiphenyl) were used as surrogate standards to evaluate the analytical efficiency. Four PCB congeners, PCB 14 and PCB 159 for the first fraction, PCB 61 for the second fraction, and PCB 204 for the third fraction, were used as internal standards to monitor the GC performance. The retention behavior of PCBs and pesticides on the PGC column are discussed. The method was found to be reproducible, effective, and reliable under the operational conditions proposed and was applied successfully to the analysis of individual PCBs and chlorinated pesticides in black-crowned night heron (Nycticorax nycticorax) egg samples.

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“…Figure 2 shows that within 80 min all 13 dioxin-like PCBs are separated on both columns, although coelution of other PCB congeners or interference during analysis of real samples is inevitable. In this case, multidimensional GC or advanced clean-up methods may be succesfully used to separate and clarify the identity of PCBs in real samples [12][13][14].…”

Section: Recovery Rates Of Coplanar Pcbs From Spiked Sand Samplesmentioning

confidence: 99%

Microwave assisted extraction and sonication of polychlorobiphenils from river sediments and risk assesment by toxic equivalency factors

Kodba

Marsel

1999

Chromatographia

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Key WordsGas chromatography Microwave and ultrasonic extraction River sediment Dioxin-like polychlorobiphenyls Toxic equivalency factors SummaryMicrowave extraction and ultrasonication of dioxin-like polychlorobiphenyls (PCBs) from sediment samples were investigated. After separation of dioxin-like PCBs from asample matrix on an acidic-alkaline silica gel column, dioxin-like PCBs were determined by GC-ECD, using dual capillary columns. Recoveries of dioxin-like PCBs in river sediment samples exceeded 80 % by both extraction techniques. Toxic equivalency factors and their use for the PCB congeners investigated were applied.

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Group separation of ortho -PCBs, coplanar non- ortho -PCBs and PCDDs/PCDFs using an alumina column as an one-step clean-up procedure

Cited by 9 publications

References 0 publications

Authentication of synthetic environmental contaminants and their (bio)transformation products in toxicology: polychlorinated biphenyls as an example

Authentication of synthetic environmental contaminants and their (bio)transformation products in toxicology: polychlorinated biphenyls as an example

Methodological Refinements in the Determination of 146 Polychlorinated Biphenyls, Including Non-Ortho- and Mono-Ortho-Substituted PCBs, and 26 Organochlorine Pesticides as Demonstrated in Heron Eggs

Microwave assisted extraction and sonication of polychlorobiphenils from river sediments and risk assesment by toxic equivalency factors

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