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Accurate analysis of trace earthy‐musty odorants in water by headspace solid phase microextraction gas chromatography‐mass spectrometry
Author(s) -
Ma Kang,
Zhang Jin Na,
Zhao Min,
He Ya Juan
Publication year - 2012
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.201200029
Subject(s) - solid phase microextraction , chemistry , chromatography , geosmin , detection limit , mass spectrometry , gas chromatography–mass spectrometry , gas chromatography , sample preparation , extraction (chemistry) , solid phase extraction , selected ion monitoring , tap water , divinylbenzene , odor , styrene , organic chemistry , environmental engineering , copolymer , engineering , polymer
A simple and sensitive method was developed for the simultaneous separation and determination of trace earthy‐musty compounds including geosmin, 2‐methylisoborneol, 2‐isobutyl‐3‐methoxypyrazine, 2‐isopropyl‐3‐methoxypyrazine, 2,3,4‐trichloroanisole, 2,4,6‐trichloroanisole, and 2,3,6‐trichloroanisole in water samples. This method combined headspace solid‐phase microextraction (HS‐SPME) with gas chromatography‐mass spectrometry and used naphthalene‐d 8 as internal standard. A divinylbenzene/carboxen/polydimethylsiloxane fiber exposing at 90°C for 30 min provided effective sample enrichment in HS‐SPME. These compounds were separated by a DB–1701MS capillary column and detected in selected ion monitoring mode within 12 min. The method showed a good linearity from 1 to 100 ng L −1 and detection limits within (0.25–0.61 ng L −1 ) for all compounds. Using naphthalene‐d 8 as the internal standard, the intra‐day relative standard deviation (RSD) was within (2.6–3.4%), while the inter‐day RSD was (3.5–4.9%). Good recoveries were obtained for tap water (80.5–90.6%), river water (81.5–92.4%), and lake water (83.5–95.2%) spiked at 10 ng L −1 . Compared with other methods using HS‐SPME for determination of odor compounds in water samples, this present method had more analytes, better precision, and recovery. This method was successfully applied for analysis of earthy‐musty odors in water samples from different sources.