顶空固相微萃取气相色谱-质谱法同时测定饮用水及其水源中4种嗅味物质  

Simultaneous determination of 4 odorants in drinking water and its source water by solid phase microextraction combine with gas chromatography-mass spectrometry

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作  者:李素芳 周娜芬 龚忆平 吴丹宁 张泾凯 吴永刚 LI Sufang;ZHOU Nafen;GONG Yiping;WU Danning;ZHANG Jingkai;WU Yonggang(Suzhou Water Supply and Drainage Monitoring Station,Suzhou 215004,China;Suzhou Jianyuan Detection Technology Co.Ltd.,Suzhou 215000,China)

机构地区:[1]苏州市供排水监测站,江苏苏州215004 [2]苏州见远检测技术有限公司,江苏苏州215000

出  处:《化学分析计量》2025年第2期108-112,共5页Chemical Analysis And Meterage

摘  要:利用顶空固相微萃取技术与气相色谱-质谱法联用,建立同时测定生活饮用水及其水源水中二甲基二硫醚、二甲基三硫醚、2-甲基异莰醇和土臭素4种嗅味物质的新方法。对比了不同材质萃取头的萃取效果,对影响萃取效果的因素氯化钠的加入量、萃取时间和温度等萃取条件进行了优化。最终确定的实验条件为向10 mL样品中加入2.0 g氯化钠,采用CAR/PDMS(85μm)萃取头,在70℃下加热30 min,并于250℃下在进样口解吸5 min。采用SIM扫描,以内标法定量,该方法4种嗅味物质的标准工作曲线线性范围为5.0~100 ng/L,相关系数均大于0.999 0,检出限为1.0 ng/L,定量限均为3.0 ng/L。进行高、中、低3种质量浓度纯水、饮用水和水源水加标回收率和精密度试验,其回收率为88.1%~105%,测定结果的相对标准偏差为0.58%~8.9%(n=7)。该方法可满足生活饮用水及其水源水的快速检测要求。与国标法相比,4种化合物的检测效率显著提升;同时,二甲基二硫醚、二甲基三硫醚灵敏度比国标法提高3倍多。A new method was developed for the simultaneous determination of dimethyl disulfide,dimethyl trisulfide,2-methylisoborneol and geosmin in drinking water and source water by headspace solid-phase microextraction combined with gas chromatography-mass spectrometry.The extraction effects of different material extraction heads were compared,and the extraction conditions such as the amount of sodium chloride added,extraction time and temperature were optimized.The final test conditions were as follows:2.0 g sodium chloride was added to 10 mL sample,CAR/PDMS(85μm)extraction head was used,heated at 70℃for 30 min,and desorbed at 250℃for 5 min.The samples were scanned by SIM and quantified by internal standard method.The standard working curves of the four odorants were 5.0-100 ng/L,and the correlation coefficients were all greater than 0.9990.The detection limit was 1.0 ng/L,and the quantitative limit was 3.0 ng/L.The recovery and precision tests of high,medium and low concentration of pure water,drinking water and source water were carried out,with a recovery rate of 88.1%-105%and a relative standard deviation of 0.58%-8.9%.This method can meet the rapid detection requirements of domestic drinking water and its source water.Compared with the national standard method,the detection efficiency of four compounds has significantly improved.Meanwhile,the sensitivity of dimethyl disulfide and dimethyl trisulfide has increased by more than three times compared to the national standard method.

关 键 词:固相微萃取法 气相色谱-质谱法 嗅味物质  

分 类 号:O657.7[理学—分析化学]

 

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