气相色谱-质谱法及嗅探技术分析蓝藻水华水体中挥发性成分  

Analysis of Volatile Compounds in Algal Bloom Water by Gas Chromatography-Mass Spectrometry and Sniffering

作　　者：虞锐鹏[1] 王利平[1] 吴胜芳[1] 车金水 刘杨岷[1] 

机构地区：[1]江南大学食品科学与技术国家重点实验室,无锡214122 [2]江南大学化学与材料工程学院,无锡214122

出　　处：《分析化学》2010年第9期1349-1352,共4页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金项目(No20707007);江苏省自然科学基金项目(NoBK2006534);江苏省科技厅大型科学仪器设备共享服务平台项目(No06-57)资助

摘　　要：采用顶空固相微萃取富集蓝藻水华水中挥发性成分,用气相色谱-质谱联用进行定性分析,对色谱峰峰面积进行归一化,计算出各成分相对百分含量,比较了不同萃取涂层、萃取温度及采样时间对分析结果的影响。确定了固相微萃取的最佳条件:CAR/PDMS涂层,萃取温度45℃,采样时间25min。鉴定出丁酸、异戊酸、乙酸、二甲基三硫、己酸、邻甲酚、丙酸、二甲基二硫、正戊酸、β-柠檬醛、硫代丁酸甲酯、3-甲基吲哚、异戊醇、甲硫醇、1-丁醇等82种化学成分。采用质谱检测器与嗅探分析器并联方式,有效鉴别得到引起人体嗅觉反感的蓝藻水华主要异味物质18种,其中二甲基三硫、二甲基二硫及β-柠檬醛为蓝藻水华暴发后增加最明显的恶臭物质。Volatile constituents of algal bloom water were investigated by headspace solid phase microextraction（HS-SPME） coupled with gas chromatography-mass spectrometry（GC-MS）.The compounds were quantified by normalization method based on chromatographic peak areas.HS-SPME parameters including different SPME fibers,extraction temperature and time were optimized.In our case,carboxen/polydimethyl-siloxane（CAR/PDMS） fiber was finally used for the extraction at 45 ℃ for 25 min.Aliquot of 82 volatile compounds were identified.The predominant components were butyric acid,isopentanoic acid,acetic acid,dimethyltrisulfide,n-hexanoic acid,o-cresol,propanoic acid,2,3-dithiobutane,pentanoic acid,beta cyclocitral,methyl thiobutyrate,3-methylindole,isopentyl alcohol,methanethiol,1-butanol etc.The GC-MS/GC-sniffering method was employed to perform the identification of the off-flavor compounds.18 kinds of smelly compounds were contained in algal bloom,in which dimethyltrisulfide,2,3-dithiobutane,and beta cyclocitral were significantly increased in the later period of algal blooms outbreak.

关 键 词：气相色谱-质谱法 嗅探分析 蓝藻水华 挥发性成分 顶空固相微萃取 

分 类 号：X830.2[环境科学与工程—环境工程]