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Automated on‐fiber derivatization with headspace SPME‐GC‐MS‐MS for the determination of primary amines in sewage sludge using pressurized hot water extraction
Author(s) -
Llop Anna,
Pocurull Eva,
Borrull Francesc
Publication year - 2011
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.201000889
Subject(s) - chemistry , chromatography , derivatization , extraction (chemistry) , sewage sludge , solid phase microextraction , gas chromatography , gas chromatography–mass spectrometry , detection limit , gas chromatography/tandem mass spectrometry , mass spectrometry , sewage , waste management , engineering
An automated, environmentally friendly, simple, selective, and sensitive method was developed for the determination of ten primary aliphatic amines in sewage sludge at μg/kg dry weight (d.w.). The procedure involves a pressurized hot water extraction (PHWE) of the analytes from the solid matrix, followed by a fully automated on‐fiber derivatization with 2,3,4,5‐pentafluorobenzaldehyde (PFBAY) and headspace solid‐phase microextraction (HS‐SPME) and subsequent gas chromatography ion‐trap tandem mass spectrometry (GC‐IT‐MS‐MS) analysis. The limits of detection (LODs) of the method were between 0.5 and 45 μg/kg (d.w.) for all compounds except for ethyl‐, isopropyl‐, and amylamine, whose LODs were 70, 109, and 116 μg/kg (d.w.), respectively. The limits of quantification (LOQs) were between 10 and 350 μg/kg (d.w.). Repeatability and intermediate precision, expressed as RSD(%) ( n =3), were lower than 18 and 21%, respectively. The method developed enabled to determine primary aliphatic amines in sludge from various urban and industrial sewage treatment plants as well as from a potable treatment plant. Most of the primary aliphatic amines were found in the sewage sludge samples analyzed corresponding to the maximum concentrations to the samples from the urban plant: for instance, isobutylamine and methylamine were found at 7728 and 12 536 μg/kg (d.w.), respectively. Amylamine was detected only in few samples but always at concentrations lower than its LOQ.