气相色谱-串联质谱法测定水中29种致嗅物质  

Determination of 29 Odor-causing Substances in Water by Gas Chromatography-Tandem Mass Spectrometry

作　　者：李丰铎 王洵[1,2] 石亚东 李涛 钱进[1,2] LI Feng-duo;WANG Xun;SHI Ya-dong;LI Tao;QIAN Jin(College of Environment,Hohai University,Nanjing 210098,China;Key Laboratory of Integrated Regulation and Resource Development on Shallow Lakes,Ministry of Education,Hohai University,Nanjing 210098,China;Taihu Basin Hydrology&Water Resources Monitoring Center(Taihu Basin Environment Monitoring Center),Wuxi 214024,China)

机构地区：[1]河海大学环境学院,江苏南京210098 [2]河海大学浅水湖泊综合治理与资源开发教育部重点实验室,江苏南京210098 [3]太湖流域水文水资源监测中心(太湖流域水环境监测中心),江苏无锡214024

出　　处：《分析测试学报》2024年第4期582-589,共8页Journal of Instrumental Analysis

基　　金：上海城投(集团)有限公司科技创新计划项目(CTKY-ZDXM-2022-001)。

摘　　要：采用顶空箭型固相微萃取(HS-Arrow-SPME)与气相色谱-串联质谱(GC-MS/MS)技术,建立了水中29种致嗅物质的快速检测方法。通过优化前处理条件和GC-MS/MS参数,选择10 mL水样加入顶空瓶中,于70℃条件下,通过3.5 g氯化钠盐析辅助预孵化8 min,然后以二乙烯基苯/羟基/聚二甲基硅氧烷(DVB/Carbon WR/PMDS)Smart SPME Arrow箭型固相萃取头萃取20 min,于240℃进样口处解吸3 min。目标物采用VF-624 MS色谱柱(30 m×0.25 mm×1.4µm)进行分离,多反应监测(MRM)模式下进行检测。结果表明,水中29种致嗅物质在5~300 ng/L范围内线性良好,相关系数(r^(2))均大于0.991,方法检出限和定量下限分别为0.31~9.27 ng/L和1.26~37.09 ng/L。以超纯水为空白基质,在10、80、160 ng/L加标水平下,各目标物的回收率为84.3%~112%,相对标准偏差(RSD,n=6)为0.10%~8.6%。该方法已用于实际水样中29种目标物的测定,可满足痕量致嗅物质的检测要求。A rapid method was developed for the determination of 29 odor-causing substances in wa⁃ter using headspace-arrow-solid-phase microextraction(HS-Arrow-SPME)coupled with gas chroma⁃tography-tandem mass spectrometry(GC-MS/MS).By optimizing the pretreatment conditions and GC-MS/MS parameters,10 mL of water samples were selected to be added into a headspace vial,pre-incubated at 70℃for 8 min with the assistance of 3.5 g NaCl salting-out,then extracted with a DVB/Carbon WR/PMDS Smart SPME Arrow extraction head for^(2)0 min,and finally desorbed at the inlet of 240℃for 3 min.The GC-MS/MS platform was configured with a VF-624 MS column(30 m×0.25 mm×1.4µm)and detected in multiple reaction monitoring(MRM)mode.The results showed that the linearity of the 29 odor-causing substances in water was good in the ranges of 5-300 ng/L with correlation coefficients(r^(2))greater than 0.991.The limits of detection and the limits of quantitation ranged of 0.31-9.27 ng/L and 1.26-37.09 ng/L,respectively.The recoveries of 29 odor-causing substances spiked with the ultra-pure water as the blank matrix at spiked levels of 10,80,and 160 ng/L were in the ranges of 84.3%-112%,and the relative standard deviations(RSDs,n=6)were in the ranges of 0.10%-8.6%.The method has been used for the determination of 29 targets in real wa⁃ter samples and can meet the requirements for the detection of trace odor-causing substances.

关 键 词：顶空箭型固相微萃取 气相色谱-串联质谱 水 致嗅物质 

分 类 号：O657.7[理学—分析化学] X132[理学—化学]