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气相色谱-串联质谱法测定水中29种致嗅物质OA北大核心CSTPCD

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

中文摘要英文摘要

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×1.4 μm)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(r2)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 20 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×1.4 μm)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(r2)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.

李丰铎;王洵;石亚东;李涛;钱进

河海大学 环境学院,江苏 南京 210098||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

化学

顶空箭型固相微萃取气相色谱-串联质谱致嗅物质

HS-Arrow-SPMEGC-MS/MSwaterodor-causing substance

《分析测试学报》 2024 (004)

582-589 / 8

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

10.12452/j.fxcsxb.23112719

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