In Situ Derivatization/Solid-Phase Microextraction: Determination of Polar Aromatic Amines
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- 作者：Thomas Zimmermann ; Wolfgang J. Ensinger ; and Torsten C. Schmidt
- 刊名：Analytical Chemistry
- 出版年：2004
- 出版时间：February 15, 2004
- 年：2004
- 卷：76
- 期：4
- 页码：1028 - 1038
- 全文大小：146K
- 年卷期：v.76,no.4(February 15, 2004)
- ISSN：1520-6882
文摘
A solid-phase microextraction GC/MS method for thetrace determination of a wide variety of polar aromaticamines in aqueous samples was developed. Prior toextraction the analytes were derivatized directly in theaqueous solution by diazotation and subsequent iodination in a one-pot reaction. The derivatives were extractedby direct-SPME using a PDMS/DVB fiber and analyzedby GC/MS in the full-scan mode. By diazotation/iodination, the polarity of the analytes was significantly decreased and as a consequence extraction yields weredramatically improved. The derivatization proved to besuitable for strongly deactivated aromatic amines and eventhe very polar diamino compounds can efficiently beenriched after derivatization. We investigated 18 anilinescomprising a wide range of functional groups, which couldbe determined simultaneously. The method was thoroughly validated, and the precision at a concentration of0.5 
g/L was 3.8-11% relative standard deviation fornonnitrated analytes using aniline-d5 as internal standardand 3.7-10% for nitroaromatic amines without internalstandard. The in situ derivatization/SPME/GC/MS methodwas calibrated over the whole analytical procedure andwas linear over 2 orders of magnitude. Using 10-mLsamples, detection limits of 2-13 ng/L were achieved for15 of the 18 analytes. For two aminodinitrotolueneisomers and a diaminonitrotoluene, detection limits rangedfrom 27 to 38 ng/L. By allowing quantification at the 0.1g/L level, analysis of all target compounds meets EUdrinking water regulations. The method provides highsensitivity, robustness, and high sample throughput byautomation. Finally, the method was applied to variousreal water samples and in wastewater from a formerammunition plant the contents of several aromatic amineswere quantified.
g/L was 3.8-11% relative standard deviation fornonnitrated analytes using aniline-d5 as internal standardand 3.7-10% for nitroaromatic amines without internalstandard. The in situ derivatization/SPME/GC/MS methodwas calibrated over the whole analytical procedure andwas linear over 2 orders of magnitude. Using 10-mLsamples, detection limits of 2-13 ng/L were achieved for15 of the 18 analytes. For two aminodinitrotolueneisomers and a diaminonitrotoluene, detection limits rangedfrom 27 to 38 ng/L. By allowing quantification at the 0.1g/L level, analysis of all target compounds meets EUdrinking water regulations. The method provides highsensitivity, robustness, and high sample throughput byautomation. Finally, the method was applied to variousreal water samples and in wastewater from a formerammunition plant the contents of several aromatic amineswere quantified.