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Výsledky výzkumu a vývoje

Publication detail

Original Title: The assessment of analgesic-residue contamination of wastewater using tandem gas chromatography with mass spectrometric detection
Czech Title: Stanovení kontaminace odpadních vod residui analgetik s použitím tandemové plynové chromatografie s hmotnostně spektrometrickou detekcí
English Title: The assessment of analgesic-residue contamination of wastewater using tandem gas chromatography with mass spectrometric detection
Author(s): LACINA, P.; MRAVCOVÁ, L.; VÁVROVÁ, M.
Type: abstract
Language: en
Original Abstract: This study is focused on determination of 10 selected drugs from the widely used group of human pharmaceuticals non-steroidal anti-inflammatory drugs (NSAID) in wastewater. Target compounds were follows: salicylic acid, acetylsalicylic acid, clofibric acid, ibuprofen, caffeine, naproxen, mefenamic acid, ketoprofen and diclofenac. Comprehensive twodimensional gas chromatography with mass spectrometric detection Time-of-Flight (GCxGCTOF MS) was used for final analysis of these compounds. Only disadvantage in this field is the necessity to derivatize selected compounds with suitable derivatization reagents. However, this work presents easy, effective and fast derivatization by silylation reagent MSTFA. Samples of wastewater were collected daily in November 2010 from the influent and effluent of WWTP in Brno Modrice in Czech Republic. Solid phase extraction (SPE) was used for extraction and preconcentration of analytes. The results of this study proves, that contamination of wastewater by human pharmaceuticals from the group on NSAID is relatively high. In addition, this study proves, that gas chromatography with mass spectrometric detection is excellent method for trace and ultratrace analysis of organic compounds, such as pharmaceuticals, due to its high separation efficiency and sensitivity. Limits of detection of this methods were ranged from 0.18 to 5 ng/L depending on specific compound. Concentrations of selected pharmaceuticals in wastewater varied from one to several tens of ug/L.
Czech abstract: Studie zaměřená na analýzu 10 vybraných zástupců léčiv ze skupiny analgetik a nesteroidních protizánětlivých látek (kyselina salicylová, kyselina acetylsalicylová, kyselina klofibrová, ibuprofen, paracetamol, kofein, naproxen, kyselina mefenamová, ketoprofen, diklofenak) v odpadní vodě. Pro finální analýzu byla použita komplexni ortogonální dvoj-dimenzionální plynová chromatografie s hmotnostě spektrometrickou detekcí Time-of-Flight (GCxGC-TOF MS). Studie současně uvádí snadnou derivatizaci cílových sloučenin pomocí silylačního činidla MSTFA. Uvedená metoda byla úspěšně aplikována na reálných vzorcích odpadní vody z čistírny odpadních vod v Brně Modřicích, odkud byly vzorky odebírány každý den jak na přítoku tak odtoku po celý měsíc listopad 2010. pro zakoncentrování a extrakci byly použita metoda extrakce tuhou fází (SPE). Výsledky studie dokazují přítomnost vybraných léčiv v odpadní vodě v poměrně vysokých koncentracích nejen na přítoku, ale v některých případech i na odtoku. Limity detekce uvedné metody se pohybovaly v rozmezí 0,18 - 5 ng/l a hodnoty koncentrací jednotlivých léčiv od jednotek do několika desítek ug/l.
English abstract: This study is focused on determination of 10 selected drugs from the widely used group of human pharmaceuticals non-steroidal anti-inflammatory drugs (NSAID) in wastewater. Target compounds were follows: salicylic acid, acetylsalicylic acid, clofibric acid, ibuprofen, caffeine, naproxen, mefenamic acid, ketoprofen and diclofenac. Comprehensive twodimensional gas chromatography with mass spectrometric detection Time-of-Flight (GCxGCTOF MS) was used for final analysis of these compounds. Only disadvantage in this field is the necessity to derivatize selected compounds with suitable derivatization reagents. However, this work presents easy, effective and fast derivatization by silylation reagent MSTFA. Samples of wastewater were collected daily in November 2010 from the influent and effluent of WWTP in Brno Modrice in Czech Republic. Solid phase extraction (SPE) was used for extraction and preconcentration of analytes. The results of this study proves, that contamination of wastewater by human pharmaceuticals from the group on NSAID is relatively high. In addition, this study proves, that gas chromatography with mass spectrometric detection is excellent method for trace and ultratrace analysis of organic compounds, such as pharmaceuticals, due to its high separation efficiency and sensitivity. Limits of detection of this methods were ranged from 0.18 to 5 ng/L depending on specific compound. Concentrations of selected pharmaceuticals in wastewater varied from one to several tens of ug/L.
Keywords: analgesics, GCxGC-TOF MS, wastewater, drug residues
Released: 24.09.2011
Location: Ioannina