分析化学2011，Vol.39Issue(12)：1823-1829,7.DOI:10.3724/SP.J.1096.2011.01823
顶空固相微萃取-气质联用测定环境水样中7种痕量土霉昧物质
Determination of Seven Musty Odor Compounds in Water by Gas Chromatography Mass Spectrometry with Headspace Solid Phase Micro-Extraction
摘要
Abstract
A method for the simultaneous determination of seven musty odor compounds [geosmin ( GSM ) , 2-methylisoborneol ( 2-MIB ) , 2-isopropyl-3-methoxypyrazine ( IPMP ) , 2-isobutyl-3-methoxypyrazine (IBMP) , 2, 4, 6-chloroanisoles(2,4, 6-TCA) , 2, 3, 6-chloroanisoles (2,3,6-TCA) and 2,3, 4-chloroanisoles(2, 3, 4-TCA) ) in water by gas chromatography-mass spectrometry (GC-MS) with headspace solid phase micro-extraction (HS/SPME) has been developed. The extraction method was absolutely solvent-free with a divinylbenzene/carboxen/polydimethylsiloxane (DVB/ CAR/PDMS) fiber used for the enrichment of analytes. To obtain the highest sensitivity, the condition parameters of HS/SPME were optimized. The final conditions were as follows: 6 g NaCl, extraction temperature of 90 ℃ , 20 mL sample volume, extraction time of 30 min and desorption time of 5 min. Selected ion monitoring (SIM) mode of GC-MS was used in quantitation. The selected ions for SIM detections were 137 m/z for IPMP, 124 m/z for IBMP, 95 m/z for 2-MIB, 195 m/z for 2,4, 6-TCA, 210 m/z for 2,3,6-TCA, 112 m/z for GSM and 210 m/z for 2,3,4-TCA. The method had linear response within (1 -100) ng/L with a correlation coefficient above 0. 997, and the detection limits (S/N=3) were below 1. 0 ng/L. The intra-day (n = 6) precision was from 1. 4% to 3. 4% and inter-day precision (m = 2, n = 6) was from 4. 2% to 6. 9%. The method was successfully applied to analyze environment water sample and the recoveries of seven compounds were in the range of (84. 0% -105. 0%) at spiked levels of (3 - 10) ng/L. The present method was compared with other methods in literature for the determination of musty odor compounds in water sample.关键词
顶空-固相微萃取/土霉味物质/气相色谱-质谱/环境水样Key words
Headspace solid phase micro-extraction/ Musty odorous compounds/ Gas chromatogra-phy/mass spectrometry/ Environment water引用本文复制引用
马康,张金娜,何雅娟,赵敏,弓爱君..顶空固相微萃取-气质联用测定环境水样中7种痕量土霉昧物质[J].分析化学,2011,39(12):1823-1829,7.基金项目
本文系水体污染控制与治理科技重大专项(No.2009ZX07420-008-02)资助 （No.2009ZX07420-008-02）
