Abstract
Mass spectrometry is a major tool for analysing organic pollutants. However, scientists often complain about laborious sample preparation. The development of new commercial high-resolution mass spectrometers gives a chance to improve simultaneously speed, reliability, and sensitivity of the analysis. Here, we used the time-of-flight high-resolution mass spectrometer Pegasus GC-HRT to identify and quantify 55 priority organic pollutants in water samples. This mass spectrometer has a high resolution of 50,000, a high mass accuracy of about 1 ppm and a very high acquisition rate of up to 200 full mass range spectra per second. 1 mL water samples were extracted with 1 mL dichloromethane. Results show that the sample preparation and analysis are achieved 30 times faster, requiring 1,000 times less water and 350 times less solvent than the classic 8270 method of the United States Environmental Protection Agency. The detection limit is 1 μg/L. The quantification limit is 10 μg/L. Our procedure, named accelerated water sample preparation, is simpler, faster, cheaper, safer and more reliable than 8270 Method.
Similar content being viewed by others
References
Alberici RM, Simas RC, Eberlin MN (2012) Ambient mass spectrometry: environmental analysis without sample preparation. In: Lebedev AT (ed) Comprehensive environmental mass spectrometry. ILM Publications, UK, pp 147–166
Bagheri H, Khalilian F, Babanezhad E, Es-haghi A, Rouini MR (2008) Modified solvent microextraction with back extraction combined with liquid chromatography-fluorescence detection for the determination of citalopram in human plasma. Anal Chim Acta 610:211–216
Ballesteros-Gomez A, Rubio S (2011) Recent advances in environmental analysis. Anal Chem 83:4579–4613
Chen X, Zhang T, Liang P, Li Y (2006) Application of continuous-flow liquid phase microextraction to the analysis of phenolic compounds in wastewater samples. Microchim Acta 155:415–420
Davey NG, Krogh ET, Gill CG (2011) Membrane-introduction mass spectrometry (MIMS). Trends Anal Chem 30:1477–1485
Eur. Union. (2002) Commission Decision 2002/657/EC implementing Council Directive 96/23/EC concerning the performance of analytical methods and the interpretation of results. Off J Eur Union 125(2002):10–32
Guo L, Liang P, Zhang T, Liu Y, Liu S (2005) Use of continuous-flow microextraction and liquid chromatography for determination of phoxim in water samples. Chromatographia 61:523–526
Harris GA, Galhena AS, Fernandez FM (2011) Ambient sampling/ionization mass spectrometry: applications and current trends. Anal Chem 83:4508–4538
He Y, Lee HK (1997) Liquid-phase microextraction in a single drop of organic solvent by using a conventional microsyringe. Anal Chem 69:4634–4640
He Y, Lee HK (2006) Continuous flow microextraction combined with high-performance liquid chromatography for the analysis of pesticides in natural waters. J Chromatogr A 1122:7–12
Huang MZ, Cheng SC, Cho YT, Shiea J (2011) Ambient ionization mass spectrometry: a tutorial. Anal Chim Acta 702:1–15
Jeannot MA, Cantwell FF (1996) Solvent microextraction into a single drop. Anal Chem 68:2236–2240
Jeannot MA, Cantwell FF (1997) Mass transfer characteristics of solvent extraction into a single drop at the tip of a syringe needle. Anal Chem 69:235–239
Jiang X, Lee HK (2004) Solvent bar microextraction. Anal Chem 76:5591–5596
Lebedev AT (2012) Comprehensive environmental mass spectrometry. ILM Publications, UK, p 510
Lebedev AT (2013) Environmental mass spectrometry. Annu Rev Anal Chem 6:163–189
Lebedev AT, Polyakova OV, Mazur DM, Artaev VB (2013) The benefits of high resolution mass spectrometry in environmental analysis. Analyst 138:6946–6953
Leong MI, Huang SD (2008) Dispersive liquid–liquid microextraction method based on solidification of floating organic drop combined with gas chromatography with electron-capture or mass spectrometry detection. J Chromatogr A 1211:8–12
Liu H, Dasgupta PK (1996) Analytical chemistry in a drop. Solvent extraction in a microdrop. Anal Chem 68:1817–1821
Liu W, Lee HK (2000) Continuous-flow microextraction exceeding 1000-fold concentration of dilute analytes. Anal Chem 72:4462–4467
Liu WL, Ko YC, Hwang BH, Li ZG, Yang TCC, Lee MR (2012) Determination of perfluorocarboxylic acids in water by ion-pair dispersive liquid–liquid microextraction and gas chromatography–tandem mass spectrometry with injection port derivatization. Anal Chim Acta 726:28–34
Ma M, Cantwell FF (1999) Chain unfolding in an ODS-bonded phase caused by the sorbed tetra-n-butylammonium ion. Anal Chem 71:388–393
Majors RE (2012) Supported liquid extraction: the best-kept secret in sample preparation. LC GC Eur 25:430–435
Method 8270D Semivolatile organic compounds by gas chromatography/mass spectrometry (GC/MS) (2007) US Environmental Protection Agency
NIST (2011). NIST/EPA/NIH Mass Spectral Database (NIST11). National Institute of Standards and Technology, part of the United States Department of Commerce, Gaithersburg, Maryland, USA. http://chemdata.nist.gov
Polyakova OV, Mazur DM, Bolshov MA, Seregina IF, Lebedev AT (2012) Estimation of contamination of atmosphere of Moscow in winter. J Anal Chem 67:1039–1049 Original Russian version (2012) in Mass-spektrometria (Rus) 9:5–15
Polyakova OV, Mazur DM, Artaev VB, Lebedev AT (2013) Determination of polycyclic aromatic hydrocarbons in water by gas chromatography/mass spectrometry with accelerated sample preparation. J Anal Chem 68:1099–1103 Original Russian version (2012) in Mass-spektrometria (Rus) 9:217–222
Przyjazny A, Kokosa JM (2002) Analytical characteristics of the determination of benzene, toluene, ethylbenzene and xylenes in water by headspace solvent microextraction. J Chromatogr A 977:143–153
Rezaee M, Assadi Y, Hosseini MRM, Aghaee E, Ahmadi F, Berijani S (2006) Determination of organic compounds in water using dispersive liquid–liquid microextraction. J Chromatogr A 1116:1–9
Schenck FJ, Hobbs JE (2004) Evaluation of the quick, easy, cheap, effective, rugged, and safe (QuEChERS) approach to pesticide residue analysis. Bull Environ Contam Toxicol 73:24–30
Takats Z, Wiseman JM, Gologan B, Cooks RG (2004) Mass spectrometry sampling under ambient conditions with desorption electrospray ionization. Science 306:471–473
Tankeviciute A, Kazlauskas R, Vickackaite V (2001) Headspace extraction of alcohols into a single drop. Analyst 126:1674–1677
Theis AL, Waldack AJ, Hansen SM, Jeannot MA (2001) Headspace solvent microextraction. Anal Chem 73:5651–5654
Vera-Avila LE, Rojo-Portillo T, Covarrubias-Herrero R, Pena-Alvarez A (2013) Capabilities and limitations of dispersive liquid–liquid microextraction with solidification of floating organic drop for the extraction of organic pollutants from water samples. Anal Chim Acta 805:60–69
Wu HF, Yen JH, Chin CC (2006) Combining drop-to-drop solvent microextraction with gas chromatography/mass spectrometry using electronic ionization and self-ion/molecule reaction method to determine methoxyacetophenone isomers in one drop of water. Anal Chem 78:1707–1712
Zanjani MRK, Yamini Y, Shariati S, Jonsson JA (2007) A new liquid-phase microextraction method based on solidification of floating organic drop. Anal Chim Acta 585:286–293
Zhu L, Tay CB, Lee HKJ (2002) Liquid–liquid–liquid microextraction of aromatic amines from water samples combined with high-performance liquid chromatography. J Chromatogr A 963:231–237
Zuloaga O, Navarro P, Bizkarguenaga E, Iparraguirre A, Vallejo A, Olivares M, Prieto A (2012) Overview of extraction, clean-up and detection techniques for the determination of organic pollutants in sewage sludge: a review. Anal Chim Acta 736:7–29
Acknowledgments
The authors would like to acknowledge LECO Corporation for allowing access to the Pegasus GC/HRT and Viatcheslav Artaev (LECO Corporation) for technical advice and support related to instrumentation used in this work and help with data processing.
Author information
Authors and Affiliations
Corresponding author
Rights and permissions
About this article
Cite this article
Polyakova, O.V., Mazur, D.M. & Lebedev, A.T. Improved sample preparation and GC–MS analysis of priority organic pollutants. Environ Chem Lett 12, 419–427 (2014). https://doi.org/10.1007/s10311-014-0464-4
Received:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s10311-014-0464-4