Abstract

There is a growing concern about the human and environmental health effects of fullerenes (e.g., C60) due to their increasing application in research, medicine, and industry. Toxicological and pharmacokinetic research requires standard methods for extraction and detection of fullerenes from biological matrices such as urine. The present study validates the use of liquid-liquid extraction (LLE) and solid-phase extraction (SPE) methods in conjunction with liquid chromatography-mass spectrometry (LC-MS) for the quantitative determination of C60 in human and synthetic urine as compared with ultrapure water. Glacial acetic acid, which is necessary to prevent emulsions during LLE, inhibited C60 detection by LC-MS, but this could be mitigated with evaporation. Aqueous C60 aggregates (nC60) were spiked at 180 μg/L into the components of a synthetic urine recipe to determine their individual impacts on extraction and detection. Urea, creatinine, and a complex protein (i.e., gelatin) were found to impair SPE, leading to a low recovery rate of 43∈±∈4% for C 60 spiked into human urine. In contrast, C60 was consistently recovered from synthetic matrices using LLE, and recovery in human urine was 80∈±∈6%. These results suggest that LLE combined with LC-MS is suitable for studying the clearance of fullerenes from the body. LLE is a robust technique that holds promise for extracting C60 from other complex biological matrices (e.g., blood, sweat, amniotic fluid) in toxicological studies, enabling a better understanding of the behavior of fullerenes in human and animal systems and facilitating a more comprehensive risk evaluation of fullerenes.

Original languageEnglish (US)
Pages (from-to)1631-1639
Number of pages9
JournalAnalytical and Bioanalytical Chemistry
Volume399
Issue number4
DOIs
StatePublished - Feb 2011

Fingerprint

Fullerenes
Liquid-Liquid Extraction
Urine
Liquid Chromatography
Liquids
Mass Spectrometry
Solid Phase Extraction
Toxicology
Liquid chromatography
Mass spectrometry
Environmental Health
Sweat
Amniotic Fluid
Gelatin
Emulsions
Research
Acetic Acid
Urea
Creatinine
Industry

Keywords

  • C
  • Chromatography
  • Environment
  • Fate
  • Mass spectrometry
  • Nano
  • Solid-phase extraction

ASJC Scopus subject areas

  • Analytical Chemistry
  • Biochemistry

Cite this

Evaluation of extraction methods for quantification of aqueous fullerenes in urine. / Benn, Troy M.; Pycke, Benny F G; Herckes, Pierre; Westerhoff, Paul; Halden, Rolf.

In: Analytical and Bioanalytical Chemistry, Vol. 399, No. 4, 02.2011, p. 1631-1639.

Research output: Contribution to journalArticle

@article{2141dc6353b44e0491b5ae2e35b998ed,
title = "Evaluation of extraction methods for quantification of aqueous fullerenes in urine",
abstract = "There is a growing concern about the human and environmental health effects of fullerenes (e.g., C60) due to their increasing application in research, medicine, and industry. Toxicological and pharmacokinetic research requires standard methods for extraction and detection of fullerenes from biological matrices such as urine. The present study validates the use of liquid-liquid extraction (LLE) and solid-phase extraction (SPE) methods in conjunction with liquid chromatography-mass spectrometry (LC-MS) for the quantitative determination of C60 in human and synthetic urine as compared with ultrapure water. Glacial acetic acid, which is necessary to prevent emulsions during LLE, inhibited C60 detection by LC-MS, but this could be mitigated with evaporation. Aqueous C60 aggregates (nC60) were spiked at 180 μg/L into the components of a synthetic urine recipe to determine their individual impacts on extraction and detection. Urea, creatinine, and a complex protein (i.e., gelatin) were found to impair SPE, leading to a low recovery rate of 43∈±∈4{\%} for C 60 spiked into human urine. In contrast, C60 was consistently recovered from synthetic matrices using LLE, and recovery in human urine was 80∈±∈6{\%}. These results suggest that LLE combined with LC-MS is suitable for studying the clearance of fullerenes from the body. LLE is a robust technique that holds promise for extracting C60 from other complex biological matrices (e.g., blood, sweat, amniotic fluid) in toxicological studies, enabling a better understanding of the behavior of fullerenes in human and animal systems and facilitating a more comprehensive risk evaluation of fullerenes.",
keywords = "C, Chromatography, Environment, Fate, Mass spectrometry, Nano, Solid-phase extraction",
author = "Benn, {Troy M.} and Pycke, {Benny F G} and Pierre Herckes and Paul Westerhoff and Rolf Halden",
year = "2011",
month = "2",
doi = "10.1007/s00216-010-4465-2",
language = "English (US)",
volume = "399",
pages = "1631--1639",
journal = "Fresenius Zeitschrift fur Analytische Chemie",
issn = "0016-1152",
publisher = "Springer Verlag",
number = "4",

}

TY - JOUR

T1 - Evaluation of extraction methods for quantification of aqueous fullerenes in urine

AU - Benn, Troy M.

AU - Pycke, Benny F G

AU - Herckes, Pierre

AU - Westerhoff, Paul

AU - Halden, Rolf

PY - 2011/2

Y1 - 2011/2

N2 - There is a growing concern about the human and environmental health effects of fullerenes (e.g., C60) due to their increasing application in research, medicine, and industry. Toxicological and pharmacokinetic research requires standard methods for extraction and detection of fullerenes from biological matrices such as urine. The present study validates the use of liquid-liquid extraction (LLE) and solid-phase extraction (SPE) methods in conjunction with liquid chromatography-mass spectrometry (LC-MS) for the quantitative determination of C60 in human and synthetic urine as compared with ultrapure water. Glacial acetic acid, which is necessary to prevent emulsions during LLE, inhibited C60 detection by LC-MS, but this could be mitigated with evaporation. Aqueous C60 aggregates (nC60) were spiked at 180 μg/L into the components of a synthetic urine recipe to determine their individual impacts on extraction and detection. Urea, creatinine, and a complex protein (i.e., gelatin) were found to impair SPE, leading to a low recovery rate of 43∈±∈4% for C 60 spiked into human urine. In contrast, C60 was consistently recovered from synthetic matrices using LLE, and recovery in human urine was 80∈±∈6%. These results suggest that LLE combined with LC-MS is suitable for studying the clearance of fullerenes from the body. LLE is a robust technique that holds promise for extracting C60 from other complex biological matrices (e.g., blood, sweat, amniotic fluid) in toxicological studies, enabling a better understanding of the behavior of fullerenes in human and animal systems and facilitating a more comprehensive risk evaluation of fullerenes.

AB - There is a growing concern about the human and environmental health effects of fullerenes (e.g., C60) due to their increasing application in research, medicine, and industry. Toxicological and pharmacokinetic research requires standard methods for extraction and detection of fullerenes from biological matrices such as urine. The present study validates the use of liquid-liquid extraction (LLE) and solid-phase extraction (SPE) methods in conjunction with liquid chromatography-mass spectrometry (LC-MS) for the quantitative determination of C60 in human and synthetic urine as compared with ultrapure water. Glacial acetic acid, which is necessary to prevent emulsions during LLE, inhibited C60 detection by LC-MS, but this could be mitigated with evaporation. Aqueous C60 aggregates (nC60) were spiked at 180 μg/L into the components of a synthetic urine recipe to determine their individual impacts on extraction and detection. Urea, creatinine, and a complex protein (i.e., gelatin) were found to impair SPE, leading to a low recovery rate of 43∈±∈4% for C 60 spiked into human urine. In contrast, C60 was consistently recovered from synthetic matrices using LLE, and recovery in human urine was 80∈±∈6%. These results suggest that LLE combined with LC-MS is suitable for studying the clearance of fullerenes from the body. LLE is a robust technique that holds promise for extracting C60 from other complex biological matrices (e.g., blood, sweat, amniotic fluid) in toxicological studies, enabling a better understanding of the behavior of fullerenes in human and animal systems and facilitating a more comprehensive risk evaluation of fullerenes.

KW - C

KW - Chromatography

KW - Environment

KW - Fate

KW - Mass spectrometry

KW - Nano

KW - Solid-phase extraction

UR - http://www.scopus.com/inward/record.url?scp=79451473490&partnerID=8YFLogxK

UR - http://www.scopus.com/inward/citedby.url?scp=79451473490&partnerID=8YFLogxK

U2 - 10.1007/s00216-010-4465-2

DO - 10.1007/s00216-010-4465-2

M3 - Article

C2 - 21153587

AN - SCOPUS:79451473490

VL - 399

SP - 1631

EP - 1639

JO - Fresenius Zeitschrift fur Analytische Chemie

JF - Fresenius Zeitschrift fur Analytische Chemie

SN - 0016-1152

IS - 4

ER -