Monitoring of four dipyrone metabolites in communal wastewater by solid phase extraction liquid chromatography electrospray ionization quadrupole time-of-flight mass spectrometry

Zsuzsa Gyenge-Szabó, N. Szoboszlai, Dávid Frigyes, G. Záray, V. Mihucz

Research output: Contribution to journalArticle

7 Citations (Scopus)

Abstract

Liquid chromatography quadrupole time-of-flight spectrometry (LC-Q-TOF-MS), equipped with electrospray ionization (ESI), was developed for the determination of the main metabolites of dipyrone - 4-aminoantipyrine (4-AA), 4-acetylaminoantipyrine (4-AAA), 4-formylaminoantipyrine (4-FAA) and 4-methylaminoantipyrine (4-MAA) in communal wastewater after reversed-phase solid phase extraction (SPE) in the low to several μg/l concentration range. Samples originated from conventional wastewater treatment plant (WWTP) using activated sewage sludge as well as from a pilot-scale WWTP operating in mixed mode (activated sewage sludge and cascade biofilms reactors with biofilms growing on fix beds and roots of greenhouse plants). Results of the present study confirmed the outcomes of our previous report according to which, 4-FAA was the most persistent metabolite, while 4-AAA and 4-MAA could be determined in the highest and lowest concentration, respectively. Moreover, the study of intraday variation of the concentration of these metabolites revealed that the concentration of 4-AA, 4-AAA and 4-FAA registered a 46%-75% increase in the samples collected at noon compared to those collected at 6 AM. Chlorination did not affect considerably the removal efficiency (about 15%) of these metabolites in samples collected for 3 months consecutively before and after disinfection. Both wastewater treatment techniques efficiently removed 4-AAA (between 80 and 96%). However, in the summer season, the removal efficiency of conventional WWTP using open-air aerated tanks is lower by 30%, (on average) than in the cold season. The concentration of the investigated metabolites showed increased concentrations in the winter season confirming the intake habits of the population from this popular analgesic and antipyretic drug.

Original languageEnglish
Pages (from-to)58-63
Number of pages6
JournalJournal of Pharmaceutical and Biomedical Analysis
Volume90
DOIs
Publication statusPublished - Mar 5 2014

Fingerprint

Dipyrone
Electrospray ionization
Solid Phase Extraction
Liquid chromatography
Metabolites
Waste Water
Liquid Chromatography
Mass spectrometry
Mass Spectrometry
Sewage
Wastewater
Wastewater treatment
Ampyrone
Monitoring
Biofilms
Sewage sludge
Antipyretics
Plant Roots
Disinfection
Chlorination

Keywords

  • Analgesic
  • Biofilm
  • Degradation
  • Disinfection
  • Metamizole

ASJC Scopus subject areas

  • Analytical Chemistry
  • Drug Discovery
  • Pharmaceutical Science
  • Spectroscopy
  • Clinical Biochemistry

Cite this

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title = "Monitoring of four dipyrone metabolites in communal wastewater by solid phase extraction liquid chromatography electrospray ionization quadrupole time-of-flight mass spectrometry",
abstract = "Liquid chromatography quadrupole time-of-flight spectrometry (LC-Q-TOF-MS), equipped with electrospray ionization (ESI), was developed for the determination of the main metabolites of dipyrone - 4-aminoantipyrine (4-AA), 4-acetylaminoantipyrine (4-AAA), 4-formylaminoantipyrine (4-FAA) and 4-methylaminoantipyrine (4-MAA) in communal wastewater after reversed-phase solid phase extraction (SPE) in the low to several μg/l concentration range. Samples originated from conventional wastewater treatment plant (WWTP) using activated sewage sludge as well as from a pilot-scale WWTP operating in mixed mode (activated sewage sludge and cascade biofilms reactors with biofilms growing on fix beds and roots of greenhouse plants). Results of the present study confirmed the outcomes of our previous report according to which, 4-FAA was the most persistent metabolite, while 4-AAA and 4-MAA could be determined in the highest and lowest concentration, respectively. Moreover, the study of intraday variation of the concentration of these metabolites revealed that the concentration of 4-AA, 4-AAA and 4-FAA registered a 46{\%}-75{\%} increase in the samples collected at noon compared to those collected at 6 AM. Chlorination did not affect considerably the removal efficiency (about 15{\%}) of these metabolites in samples collected for 3 months consecutively before and after disinfection. Both wastewater treatment techniques efficiently removed 4-AAA (between 80 and 96{\%}). However, in the summer season, the removal efficiency of conventional WWTP using open-air aerated tanks is lower by 30{\%}, (on average) than in the cold season. The concentration of the investigated metabolites showed increased concentrations in the winter season confirming the intake habits of the population from this popular analgesic and antipyretic drug.",
keywords = "Analgesic, Biofilm, Degradation, Disinfection, Metamizole",
author = "Zsuzsa Gyenge-Szab{\'o} and N. Szoboszlai and D{\'a}vid Frigyes and G. Z{\'a}ray and V. Mihucz",
year = "2014",
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doi = "10.1016/j.jpba.2013.11.019",
language = "English",
volume = "90",
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T1 - Monitoring of four dipyrone metabolites in communal wastewater by solid phase extraction liquid chromatography electrospray ionization quadrupole time-of-flight mass spectrometry

AU - Gyenge-Szabó, Zsuzsa

AU - Szoboszlai, N.

AU - Frigyes, Dávid

AU - Záray, G.

AU - Mihucz, V.

PY - 2014/3/5

Y1 - 2014/3/5

N2 - Liquid chromatography quadrupole time-of-flight spectrometry (LC-Q-TOF-MS), equipped with electrospray ionization (ESI), was developed for the determination of the main metabolites of dipyrone - 4-aminoantipyrine (4-AA), 4-acetylaminoantipyrine (4-AAA), 4-formylaminoantipyrine (4-FAA) and 4-methylaminoantipyrine (4-MAA) in communal wastewater after reversed-phase solid phase extraction (SPE) in the low to several μg/l concentration range. Samples originated from conventional wastewater treatment plant (WWTP) using activated sewage sludge as well as from a pilot-scale WWTP operating in mixed mode (activated sewage sludge and cascade biofilms reactors with biofilms growing on fix beds and roots of greenhouse plants). Results of the present study confirmed the outcomes of our previous report according to which, 4-FAA was the most persistent metabolite, while 4-AAA and 4-MAA could be determined in the highest and lowest concentration, respectively. Moreover, the study of intraday variation of the concentration of these metabolites revealed that the concentration of 4-AA, 4-AAA and 4-FAA registered a 46%-75% increase in the samples collected at noon compared to those collected at 6 AM. Chlorination did not affect considerably the removal efficiency (about 15%) of these metabolites in samples collected for 3 months consecutively before and after disinfection. Both wastewater treatment techniques efficiently removed 4-AAA (between 80 and 96%). However, in the summer season, the removal efficiency of conventional WWTP using open-air aerated tanks is lower by 30%, (on average) than in the cold season. The concentration of the investigated metabolites showed increased concentrations in the winter season confirming the intake habits of the population from this popular analgesic and antipyretic drug.

AB - Liquid chromatography quadrupole time-of-flight spectrometry (LC-Q-TOF-MS), equipped with electrospray ionization (ESI), was developed for the determination of the main metabolites of dipyrone - 4-aminoantipyrine (4-AA), 4-acetylaminoantipyrine (4-AAA), 4-formylaminoantipyrine (4-FAA) and 4-methylaminoantipyrine (4-MAA) in communal wastewater after reversed-phase solid phase extraction (SPE) in the low to several μg/l concentration range. Samples originated from conventional wastewater treatment plant (WWTP) using activated sewage sludge as well as from a pilot-scale WWTP operating in mixed mode (activated sewage sludge and cascade biofilms reactors with biofilms growing on fix beds and roots of greenhouse plants). Results of the present study confirmed the outcomes of our previous report according to which, 4-FAA was the most persistent metabolite, while 4-AAA and 4-MAA could be determined in the highest and lowest concentration, respectively. Moreover, the study of intraday variation of the concentration of these metabolites revealed that the concentration of 4-AA, 4-AAA and 4-FAA registered a 46%-75% increase in the samples collected at noon compared to those collected at 6 AM. Chlorination did not affect considerably the removal efficiency (about 15%) of these metabolites in samples collected for 3 months consecutively before and after disinfection. Both wastewater treatment techniques efficiently removed 4-AAA (between 80 and 96%). However, in the summer season, the removal efficiency of conventional WWTP using open-air aerated tanks is lower by 30%, (on average) than in the cold season. The concentration of the investigated metabolites showed increased concentrations in the winter season confirming the intake habits of the population from this popular analgesic and antipyretic drug.

KW - Analgesic

KW - Biofilm

KW - Degradation

KW - Disinfection

KW - Metamizole

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