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Analysis of polynitrophenols and hexyl by liquid chromatography–mass spectrometry using atmospheric pressure ionisation methods and a volatile ion-pairing reagent

Pamme, Nicole and Steinbach, Klaus and Ensinger, Wolfgang and Schmidt, Torsten C. (2002):
Analysis of polynitrophenols and hexyl by liquid chromatography–mass spectrometry using atmospheric pressure ionisation methods and a volatile ion-pairing reagent.
In: Journal of Chromatography A, pp. 47-54, 943, (1), ISSN 00219673,
[Online-Edition: http://dx.doi.org/10.1016/S0021-9673(01)01430-3],
[Article]

Abstract

An LC–MS method for the determination of picric acid (2,4,6-trinitrophenol), its reductive transformation products picramic acid (2-amino-4,6-dinitrophenol) and iso-picramic acid (4-amino-2,6-dinitrophenol) and hexyl (2,2′,4,4′,6,6′-hexanitrodiphenylamine) has been developed. The analytes were separated using ion-pairing chromatography with a volatile ion-pairing reagent suitable for subsequent MS detection. The performance of an atmospheric pressure chemical ionisation (APCI) and an electrospray ionisation (ESI) interface was compared. ESI-MS is more sensitive for the analytes, especially for hexyl and picric acid, APCI-MS delivered more fragments necessary for unequivocal identification. With LC–ESI-MS limits of detection using single ion monitoring (SIM) mode are 4 ng (iso-picramic acid), 800 pg (picramic acid), 400 pg (picric acid) and 80 pg (hexyl). For quantification, 15N-picric acid was used as an internal standard. Using this new method, the degradation of picric acid in soil was monitored in a laboratory study. Furthermore, the presence of picramic acid was for the first time verified in soil samples from a former ammunition plant.

Item Type: Article
Erschienen: 2002
Creators: Pamme, Nicole and Steinbach, Klaus and Ensinger, Wolfgang and Schmidt, Torsten C.
Title: Analysis of polynitrophenols and hexyl by liquid chromatography–mass spectrometry using atmospheric pressure ionisation methods and a volatile ion-pairing reagent
Language: English
Abstract:

An LC–MS method for the determination of picric acid (2,4,6-trinitrophenol), its reductive transformation products picramic acid (2-amino-4,6-dinitrophenol) and iso-picramic acid (4-amino-2,6-dinitrophenol) and hexyl (2,2′,4,4′,6,6′-hexanitrodiphenylamine) has been developed. The analytes were separated using ion-pairing chromatography with a volatile ion-pairing reagent suitable for subsequent MS detection. The performance of an atmospheric pressure chemical ionisation (APCI) and an electrospray ionisation (ESI) interface was compared. ESI-MS is more sensitive for the analytes, especially for hexyl and picric acid, APCI-MS delivered more fragments necessary for unequivocal identification. With LC–ESI-MS limits of detection using single ion monitoring (SIM) mode are 4 ng (iso-picramic acid), 800 pg (picramic acid), 400 pg (picric acid) and 80 pg (hexyl). For quantification, 15N-picric acid was used as an internal standard. Using this new method, the degradation of picric acid in soil was monitored in a laboratory study. Furthermore, the presence of picramic acid was for the first time verified in soil samples from a former ammunition plant.

Journal or Publication Title: Journal of Chromatography A
Volume: 943
Number: 1
Uncontrolled Keywords: Nitrophenols, Hexyl, Picric acid, Picramic acid, Isopicramic acid
Divisions: 11 Department of Materials and Earth Sciences > Material Science > Material Analytics
11 Department of Materials and Earth Sciences > Material Science
11 Department of Materials and Earth Sciences
Date Deposited: 26 Jun 2012 07:25
Official URL: http://dx.doi.org/10.1016/S0021-9673(01)01430-3
Identification Number: doi:10.1016/S0021-9673(01)01430-3
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