The Rate of Success of the Accelerated Solvent Extraction (Ase) of Fat and Organochlorine Pesticides from Dried Fish Meat Samples

The replacement of conventional sample preparation techniques with newer techniques which are automated, faster and more eco-friendly, is nowadays desired in every analytical laboratory. One of the techniques with the attributes mentioned above is the Accelerated Solvent Extraction. In order to evaluate how successful this method is for the extraction of fat and organochlorine pesticides (OCPs) from dried fish meat samples, we have tested two series of diverse fish using Dionex™ 350 ASE provided by Thermo Scientific™ (Germany). For a more interesting approach, we added to our investigation 7 polychlorinated biphenyl (PCBs), 3 thricholorobenzenes, 2 tetrachlorobenzenes, 1 pentachlorobenzenes and 2,3,7,8-tetrachlorodibenzo-p-dioxin (TCDD). The study focused on comparing the recoveries of these analytes from different fish samples, after replacing the conventional reference method of the laboratory with ASE. The ASE parameters tested were previously used for the extraction of fat and polybrominated diphenyl ethers (PBDE) from fish samples: temperature: 120 ° C; static time: 5 min; number of cycles: 3; flushing volume: 25%; rinse with nitrogen: 90 s; solvent: cyclohexane/ethyl acetate (ratio 1:1). The ASE method provided similar and in some cases better results when compared to the standard reference method, more rapidly, eco-friendly and safer. Any high or low recoveries of the analytes taken into study are attributed to random or systematic errors during the Clean-up step of the extracts and the quantification with Gas Chromatography coupled with Tandem Mass-Spectrometry (GC MS/MS)

The Development of an Automated Clean-up for Fat Extracts in the Routine Analysis of Organochlorine Compounds in Fish Meat

The present work describes the development of a new, automatic High Performance Liquid Chromatography (HPLC) Clean-up step, in the methodology of sample preparation and multi-residue determination of organochlorine compounds (OCs) in fish meat. 24 OCs were taken into study. In addition 7 Polychlorinated Biphenyls (PCBs), 7 chlorobenzene compounds and one 2,3,7,8-Tetrachlorodibenzo-p-dioxin (TCDD) were investigated. The HPLC conditions were established in accordance with the validated traditional Clean-up step of the laboratory. The technique was applied on a dilution of analytes of interest in order to establish the period of time in which the compounds are eluted. Another set of experiments involved fish oil, in order to identify and separate the fat fraction from the analytes. To confirm the findings of the experiments mentioned above, extracts of fish samples obtained after Accelerated Solvent Extraction (ASE) were examined. The samples were spiked with the analytes of interest before HPLC clean-up step and quantified through Gas Chromatography coupled with tandem Mass Spectrometry (GC-MS/MS). A HPLC clean-up technique lasting 38 minutes/sample was developed. The method is not suitable for OCs such as Endosulfansulfat and Endrine Ketone due to the very low recovery results.Â

Trace determination of the flame retardant tetrabromobisphenol A in the atmosphere by gas chromatography–mass spectrometry

A simple and effective method has been developed for analysis of the flame retardant tetrabromobisphenol A (TBBPA) in environmental samples by using modified soxhlet extraction in combination with silica gel clean-up, derivatization with silylation reagent and gas chromatography–mass spectrometry (GC–MS) in selected ion monitoring mode (SIM). Satisfactory recoveries were achieved for the large volume sampling, soxhlet extraction and silica gel clean-up. The overall recovery is 79 ± 1%. The derivatization procedure is simple and fast, and produces stable TBBPA derivative. GC–MS with electronic impact (EI) ionization mode shows better detection power than using negative chemical ionization (NCI) mode. EI gives a method detection limit of 0.04 pg m−3 and enables to determine trace TBBPA in ambient air in remote area. The method was successfully applied to the determination of TBBPA in atmospheric samples collected over land and coastal regions. The concentrations of TBBPA ranged from below the method detection limit (0.04 pg m−3) to 0.85 pg m−3. A declining trend with increasing latitude was present from the Wadden Sea to the Arctic. The atmospheric occurrence of TBBPA in the Arctic is significant and might imply that TBBPA has long-range transport potential

The Development of an Automated Clean-up for Fat Extracts in the Routine Analysis of Organochlorine Compounds in Fish Meat

The present work describes the development of a new, automatic High Performance Liquid Chromatography (HPLC) Clean-up step, in the methodology of sample preparation and multi-residue determination of organochlorine compounds (OCs) in fish meat. 24 OCs were taken into study. In addition 7 Polychlorinated Biphenyls (PCBs), 7 chlorobenzene compounds and one 2,3,7,8-Tetrachlorodibenzo-p-dioxin (TCDD) were investigated. The HPLC conditions were established in accordance with the validated traditional Clean-up step of the laboratory. The technique was applied on a dilution of analytes of interest in order to establish the period of time in which the compounds are eluted. Another set of experiments involved fish oil, in order to identify and separate the fat fraction from the analytes. To confirm the findings of the experiments mentioned above, extracts of fish samples obtained after Accelerated Solvent Extraction (ASE) were examined. The samples were spiked with the analytes of interest before HPLC clean-up step and quantified through Gas Chromatography coupled with tandem Mass Spectrometry (GC-MS/MS). A HPLC clean-up technique lasting 38 minutes/sample was developed. The method is not suitable for OCs such as Endosulfansulfat and Endrine Ketone due to the very low recovery results.

The Rate of Success of the Accelerated Solvent Extraction (Ase) of Fat and Organochlorine Pesticides from Dried Fish Meat Samples

The replacement of conventional sample preparation techniques with newer techniques which are automated, faster and more eco-friendly, is nowadays desired in every analytical laboratory. One of the techniques with the attributes mentioned above is the Accelerated Solvent Extraction. In order to evaluate how successful this method is for the extraction of fat and organochlorine pesticides (OCPs) from dried fish meat samples, we have tested two series of diverse fish using Dionex™ 350 ASE provided by Thermo Scientific™ (Germany). For a more interesting approach, we added to our investigation 7 polychlorinated biphenyl (PCBs), 3 thricholorobenzenes, 2 tetrachlorobenzenes, 1 pentachlorobenzenes and 2,3,7,8-tetrachlorodibenzo-p-dioxin (TCDD). The study focused on comparing the recoveries of these analytes from different fish samples, after replacing the conventional reference method of the laboratory with ASE. The ASE parameters tested were previously used for the extraction of fat and polybrominated diphenyl ethers (PBDE) from fish samples: temperature: 120 ° C; static time: 5 min; number of cycles: 3; flushing volume: 25%; rinse with nitrogen: 90 s; solvent: cyclohexane/ethyl acetate (ratio 1:1). The ASE method provided similar and in some cases better results when compared to the standard reference method, more rapidly, eco-friendly and safer. Any high or low recoveries of the analytes taken into study are attributed to random or systematic errors during the Clean-up step of the extracts and the quantification with Gas Chromatography coupled with Tandem Mass-Spectrometry (GC MS/MS)

Methodologies and Results Concerning the Determination of Ocs And Pcbs From Fish Meat

In the last decade, studies have been focusing on determinations of persistent organic pollutants (POPs), well known for being involved in human chronic diseases. Various approaches and methodologies are used in monitoring these chemical substances in fish food chain. Therefore, their development, functionality and efficiency are vital for consumers’ protection. The aim of this paper is to review recently published analytical techniques for sample preparation in the determination of POP residues such as organochlorine compounds (OCs) and polychlorinated biphenyls (PCBs). Limitations and advantages of sample preparation techniques are discussed and compared so that they can facilitate the decision of future analysts upon adequate protocols in individual laboratories. A list of the most common compounds quantified nowadays is displayed. In addition, results achieved in original papers are used to briefly describe the current situation on different continents, with third world countries undergoing more pollution than the rest of the world

Aerobic nonylphenol degradation and nitro-nonylphenol formation by microbial cultures from sediments

Nonylphenol (NP) is an estrogenic pollutant which is widely present in the aquatic environment. Biodegradation of NP can reduce the toxicological risk. In this study, aerobic biodegradation of NP in river sediment was investigated. The sediment used for the microcosm experiments was aged polluted with NP. The biodegradation of NP in the sediment occurred within 8 days with a lag phase of 2 days at 30°C. During the biodegradation, nitro-nonylphenol metabolites were formed, which were further degraded to unknown compounds. The attached nitro-group originated from the ammonium in the medium. Five subsequent transfers were performed from original sediment and yielded a final stable population. In this NP-degrading culture, the microorganisms possibly involved in the biotransformation of NP to nitro-nonylphenol were related to ammonium-oxidizing bacteria. Besides the degradation of NP via nitro-nonylphenol, bacteria related to phenol-degrading species, which degrade phenol via ring cleavage, are abundantly present