Abstract
A rapid, sensitive, and cost-effective analytical method was developed for the analysis of selected semi-volatile organic compounds in water. The method used an automated online solid-phase extraction technique coupled with programmed-temperature vaporization large-volume injection gas chromatography/mass spectrometry. The water samples were extracted by using a fully automated mobile rack system based on x-y-z robotic techniques using syringes and disposable 96-well extraction plates. The method was validated for the analysis of 30 semivolatile analytes in drinking water, groundwater, and surface water. For a sample volume of 10 mL, the linear calibrations ranged from 0.01 or 0.05 to 2.5 μg·L−1, and the method detection limits were less than 0.1 μg·L−1. For the reagent water samples fortified at 1.0 μg·L−1 and 2.0 μg·L−1, the obtained mean absolute recoveries were 70%–130% with relative standard deviations of less than 20% for most analytes. For the drinking water, groundwater, and surface water samples fortified at 1.0 μg·L−1, the obtained mean absolute recoveries were 50%–130% with relative standard deviations of less than 20% for most analytes. The new method demonstrated three advantages: 1) no manipulation except the fortification of surrogate standards prior to extraction; 2) significant cost reduction associated with sample collection, shipping, storage, and preparation; and 3) reduced exposure to hazardous solvents and other chemicals. As a result, this new automated method can be used as an effective approach for screening and/or compliance monitoring of selected semi-volatile organic compounds in water.
Similar content being viewed by others
References
Lacorte S, Guiffard I I, Fraisse D, Barceló D. Broad spectrum analysis of 109 priority compounds listed in the 76/464/CEE Council Directive using solid-phase extraction and GC/EI/MS. Analytical Chemistry, 2000, 72(7): 1430–1440
Tomkins B A, Griest W H. Determinations of N-nitrosodimethylamine at part-per-trillion concentrations in contaminated groundwaters and drinking waters featuring carbon-based membrane extraction disks. Analytical Chemistry, 1996, 68(15): 2533–2540
Li N, Lee H K. Sample preparation based on dynamic ion-exchange solid-phase extraction for GC/MS analysis of acidic herbicides in environmental waters. Analytical Chemistry, 2000, 72(14): 3077–3084
Dombrowski T R, Wilson G S, Thurman E M. Investigation of anion-exchange and immunoaffinity particle-loaded membranes for the isolation of charged organic analytes from water. Analytical Chemistry, 1998, 70(9): 1969–1978
Winslow S D, Prakash B, Domino M M, Pepich B V, Munch D J. Determination of Selected Semivolatile Organic Compounds in Drinking Water by Solid Phase Extraction and Capillary Column Gas Chromatography/Mass Spectrometry (GC/MS), Method 526 Revision 1.0, United States Environmental Protection Agency, 2000, http://www.epa.gov/safewater/methods/pdfs/526.pdf
Price E K, Prakash B, Domino M M, Pepich B V, Munch D J. Determination of Selected Pesticides and Flame Retardants in Drinking Water by Solid Phase Extraction and Capillary Column Gas Chromatography/Mass Spectrometry (GC/MS), Method 527 Revision. 1.0, United States Environmental Protection Agency, 2005, http://www.epa.gov/safewater/methods/pdfs/527.pdf
Munch J W. Determination of Phenols in Drinking Water by Solid Phase Extraction and Capillary Column Gas Chromatography/Mass Spectrometry (GC/MS), Method 528 Revision 1.0, United States Environmental Protection Agency, 2000, http://www.epa.gov/nerlcwww/m_528.pdf
Munch J W. Determination of Explosives and Related Compounds in Drinking Water by Solid Phase Extraction and Capillary Column Gas Chromatography/Mass Spectrometry (GC/MS), Method 529 Revision 1.0, United States Environmental Protection Agency, 2002, http://www.epa.gov/nerlcwww/m_529.pdf
Munch J W, Bassett M V. Determination of Nitrosamines in Drinking Water by Solid Phase Extraction and Capillary Column Gas Chromatography with Large Volume Injection and Chemical Ionization tandem mass spectrometry (MS/MS), Method 521 Version 1.0, United States Environmental Protection Agency, 2004, http://www.epa.gov/nerlcwww/m_521.pdf
Eichelberger J W, Behymer T D, Budde W L. Determination of Organic Compounds in Drinking Water by Liquid-Solid Extraction and Capillary Column Gas Chromatography/Mass Spectrometry, Method 525.2 Revision 2.0, United States Environmental Protection Agency, 1995, http://www.epa.gov/ogwdw/methods/epachem.html
Quintana J B, Reemtsma T. Sensitive determination of acidic drugs and triclosan in surface and wastewater by ion-pair reverse-phase liquid chromatography/tandem mass spectrometry. Rapid Communications in Mass Spectrometry, 2004, 18(7): 765–774
Smith G A, Lloyd T L. Automated solid-phase extraction and sample preparation — Finding the right solution for your laboratory, LC·GC, 1998, 16(5): S22–S31
Parker III T D, Wright D S, Rossi D T. Design and evaluation of an automated solid-phase extraction method development system for use with biological fluids. Analytical Chemistry, 1996, 68(14): 2437–2441
Hyötyläinen T, Riekkola M. Direct coupling of reversed-phase liquid chromatography to gas chromatography. Journal of Chromatography A, 1998, 819(1–2): 13–24
Mol H G J, Janssen H G, Cramers C A, Vreuls J J, Brinkman U A Th. Trace level analysis of micropollutants in aqueous samples using gas chromatography with on-line sample enrichment and large volume injection. Journal of Chromatography A, 1995, 703(1–2): 277–307
Rinkema F D, Louter A J H, Brinkman U A Th. Large-volume injections in gas chromatography-atomic emission detection: an approach for trace-level detection in water analysis. Journal of Chromatography A, 1994, 678(2): 289–297
Mol H G J, Althuizen M, Janssen H G, Cramers C A, Brinkman U A Th. Environmental applications of large volume injection in capillary GC using PTV injectors. Journal of High Resolution Chromatography, 1996, 19(2): 69–79
Engewald W, Teske J, Efer J. Programmed temperature vaporisers-based large volume injection in capillary gas chromatography. Journal of Chromatography A, 1999, 842(1–2): 143–161
van Hout MWJ, de Zeeuw R A, Franke J P, de Jong G J. Evaluation of the programmed temperature vaporiser for large-volume injection of biological samples in gas chromatography. Journal of Chromatography B, Analytical Technologies in the Biomedical and Life Sciences, 1999, 729(1–2): 199–210
Arnold C G, Berg M, Müller S R, Dommann U, Schwarzenbach R P. Determination of organotin compounds in water, sediments, and sewage sludge using perdeuterated internal standards, accelerated solvent extraction, and large-volume-injection GC/MS. Analytical Chemistry, 1998, 70(14): 3094–3101
Öllers S, van Lieshout M, Janssen H, Cramers C A. Development of an interface for directly coupled solid-phase extraction and GC-MS analysis, LC·GC, 1997, 15(9): 847–852
René G, van der Hoff G R, Gort S M, Baumann R A, van Zoonen P. Clean-up of some organochlorine and pyrethroid insecticides by automated solid-phase extraction cartridges coupled to capillary GC-ECD. Journal of High Resolution Chromatography, 1991, 14(7): 465–470
Dallüge J, Hankemeier Th, Vreuls R J J, Brinkman U A Th. On-line coupling of immunoaffinity-based solid-phase extraction and gas chromatography for the determination of s-triazines in aqueous samples. Journal of Chromatography A, 1999, 830(2): 377–386
Brinkman U A Th, Hankemeier Th, Vreuls R J J. On-line solid-Phase extraction-capillary gas chromatography for water analysis. Chemical Analysis (Warsaw), 1995, 40: 495–509
Li Y, George J E, McCarty C L. Online in situ analysis of selected semi-volatile organic compounds in water by automated microscale solid-phase extraction with large-volume injection/gas chromatography/mass spectrometry. Journal of Chromatography A, 2007, 1176(1–2): 223–230
Glasser J A, Forest D L, McKee G D, Quave S A, Budde W L. Trace analyses for wastewaters. Environmental Science & Technology, 1981, 15(12): 1426–1435
Author information
Authors and Affiliations
Corresponding author
Rights and permissions
About this article
Cite this article
Li, Y., McCarty, C.L. & George, E.J. Determination of selected semi-volatile organic compounds in water using automated online solid-phase extraction with large-volume injection/gas chromatography/mass spectrometry. Front. Environ. Sci. Eng. China 5, 417–425 (2011). https://doi.org/10.1007/s11783-011-0310-x
Received:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s11783-011-0310-x