上海市环境科学研究院,上海 200233
周 铭,高级工程师,研究方向:环境分析与检测,E-mail:zm_jeff@163.com
收稿:2025-09-17,
修回:2026-02-06,
录用:2026-03-06,
网络首发:2026-03-23,
纸质出版:2026-05-15
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陈秀雯,王磊,柯天英,赵俊明,周铭.顶空箭型固相微萃取/气相色谱-三重四极杆质谱法同时测定地表水中64种异味物质[J].分析测试学报,2026,45(05):1-9.
CHEN Xiu-wen,WANG Lei,KE Tian-ying,ZHAO Jun-ming,ZHOU Ming.Simultaneous Determination of 64 Odor-causing Substances in Surface Water by Headspace Arrow Solid-phase Microextraction/Gas Chromatography-Triple Quadrupole Mass Spectrometry[J].Journal of Instrumental Analysis,2026,45(05):1-9.
陈秀雯,王磊,柯天英,赵俊明,周铭.顶空箭型固相微萃取/气相色谱-三重四极杆质谱法同时测定地表水中64种异味物质[J].分析测试学报,2026,45(05):1-9. DOI: 10.12452/j.fxcsxb.25091702.
CHEN Xiu-wen,WANG Lei,KE Tian-ying,ZHAO Jun-ming,ZHOU Ming.Simultaneous Determination of 64 Odor-causing Substances in Surface Water by Headspace Arrow Solid-phase Microextraction/Gas Chromatography-Triple Quadrupole Mass Spectrometry[J].Journal of Instrumental Analysis,2026,45(05):1-9. DOI: 10.12452/j.fxcsxb.25091702.
针对地表水异味问题,建立了基于顶空箭型固相微萃取/气相色谱-三重四极杆质谱的地表水中64种异味物质同时测定方法,涉及多个类别的藻源及工业源典型异味物质。通过单因素实验,优化固相微萃取头种类、萃取时间、萃取温度、孵化时间、氯化钠加入量等参数。得到最佳条件为:在5.0 mL样品中加入1.80 g氯化钠,60 ℃下孵化5 min后,插入DVB/CAR/ PDMS固相微萃取头,萃取30 min。64种异味物质的检出限为0.92~29.06 ng/L,线性范围为5.0~2 000 ng/L,相关系数(
r
2
)均大于0.990。3个加标浓度下的平均回收率为60.1%~134%,相对标准偏差为1.8%~21%。采用该法检测上海市5个地表水样品,分别检出二甲硫醚(5.13~18.04 ng/L)、甲硫醇(6.58~25.12 ng/L)和2-甲基异莰醇(11.13~11.42 ng/L)。该方法前处理自动化,可用于地表水中异味物质的高通量快速筛查。
To address the odor issue in surface water,a method for the simultaneous determination of 64 odor-causing substances in surface water was established based on headspace arrow solid-phase microextraction coupled with gas chromatography-triple quadrupole mass spectrometry(HS-SPME Arrow/GC-MS/MS). The targeted odor-causing substances cover multiple categories,including typical algal-derived and industrial-derived ones such as sulfides/thiols,halohydrocarbons/aromatic hydrocarbons,terpenes,pyrazines,esters,phenols,aldehydes and ketones,ethers,and amines. Single-factor experiments were conducted to investigate the effects of parameters,including SPME fiber type,extraction time,extraction temperature,incubation time,and sodium chloride(NaCl) addition amount,on the extraction efficiency of the 64 odor-causing substances. The results indicated that the optimal conditions were as follows:after introducing 1.80 g NaCl to 5.0 mL solution,the bottle was incubated for 5 min at 60 ℃,then a DVB/CAR/PDMS(divinylbenzene/carboxen/ polydimethylsiloxane) SPME fiber was used for the ex
traction for 30 min.The limits of detection for the 64 odor-causing substances ranged from 0.92 to 29.06 ng/L,with all linear correlation coefficients(
r
2
) greater than 0.990 in the linear range of 5.0-2 000 ng/L. At three spiked concentration levels,the average spiked recoveries ranged from 60.1% to 134%,and the relative standard deviations(RSDs) varied between 1.8% and 21%. When this method was used to detect 5 surface water samples from Shanghai,methyl sulfide(5.13-18.04 ng/L),methanethiol(6.58-25.12 ng/L),and 2-methylisoborneol(2-MIB,11.13-11.42 ng/L) were detected,respectively.This method is characterized by automated sample pretreatment,and can be applied to the high-throughput rapid screening of odor-causing substances in surface water.
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