箭型顶空固相微萃取-三重四极杆气质联用法测定水中2种环状缩醛(2-EMD、2-EDD)、2-甲基异莰醇和土臭素  

Determination of Two Cyclic Acetals(2-EMD,2-EDD),2-Methylisoborneol and Geosmin in Water by Headspace SPME Arrow Combined with Gas Chromatography-Triple Quadrupole Mass Spectrometry

作　　者：李冰 LI Bing(Shanghai Water Supply Dispatching and Monitoring Center,Shanghai 200002,China)

机构地区：[1]上海市供水调度监测中心,上海200002

出　　处：《净水技术》2023年第11期191-199,共9页Water Purification Technology

基　　金：上海市2019年度“科技创新行动计划”:基于市政自来水直饮目标的上海市水安全计划与直饮水实施策略研究(19DZ1204402)。

摘　　要：采用箭型自动顶空固相微萃取(SPME Arrow)技术,对水中的2-甲基异莰醇(2-MIB)、土臭素(GSM)、2-乙基-4-甲基-1,3-二氧戊环(2-EMD)、2-乙基-5,5-二甲基-1,3-二氧六环(2-EDD)进行吸附,进入三重四极杆气质联用系统定量分析,重点针对萃取温度、盐析剂浓度、转子速率、进样深度、萃取时间等条件进行了优化。优化后的条件:萃取温度为40℃、盐析剂质量分数为20%、转子速率为500 r/min、进样深度为65 mm、顶空萃取时间为35 min,在250℃下解吸5 min后进入三重四极杆气质联用仪进行分析。该方法检测的4种化合物线性较好,R^(2)>0.995,方法准确度高、重复性好,实际水样分别加标10、50、100 ng/L,均进行6次重复测定。4种化合物的相对标准偏差最大为7.06%,加标回收率为89.96%~113.01%,方法检出限为0.7~1.0 ng/L,低于各物质的嗅阈值。该方法可以用来快速检测实际水样中的嗅味物质。Headspace solid-phase micro-extraction(SPME)Arrow technology was used to adsorb 2-methylisoborneol(2-MIB),geosmin(GSM),2-ethyl-4-methyl-1,3-dioxolane(2-EMD),2-ethyl-5,5-dimethyl-1,3-dioxane(2-EDD)in water,and entering gas chromatography-triple quadrupole mass spectrometry system for quantitative analysis afterwards.The article focuses on the optimization in extraction temperature,salting-out agent concentration,agitator speed,inlet penetration depth and extraction time.The optimized conditions were as follows:extraction temperature was 40℃,mass fraction of salting-out agent was 20%,agitator speed was 500 r/min,inlet penetration depth was 65 mm,extraction time was 35 min,desorbed at 250℃for 5 min in gas chromatography-triple quadrupole mass spectrometry system for analysis.The linear correlation coefficients of the 4 compounds detected by this method are all greater than 0.995.The method has high accuracy and good repeatability.The water samples were spiked with 10,50,100 ng/L respectively,and all the measurements were repeated for 6 times.The maximum relative standard deviation of the four compounds was 7.06%,and the recoveries were 89.96%~113.01%.The detection limits of the method were 0.7~1.0 ng/L,which was lower than the odor threshold of each compound.This method can be used to detect odorous compounds in water samples efficiently.

关 键 词：箭型自动顶空固相微萃取 三重四极杆气质联用 嗅味物质 2-乙基-4-甲基-1 3-二氧戊环 2-乙基-5 5-二甲基-1 3-二氧六环 

分 类 号：R123[医药卫生—环境卫生学]