首页|期刊导航|分析测试学报|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

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OA

Simultaneous Determination of 64 Odor-causing Substances in Surface Water by Headspace Arrow Solid-phase Microextraction/Gas Chromatography-Triple Quadrupole Mass Spectrometry

中文摘要英文摘要

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(r2)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 typi‑cal algal-derived and industrial-derived ones such as sulfides/thiols,halohydrocarbons/aromatic hy‑drocarbons,terpenes,pyrazines,esters,phenols,aldehydes and ketones,ethers,and amines.Single-factor experiments were conducted to investigate the effects of parameters,including SPME fi‑ber 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 indicat‑ed 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 extraction 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 coeffi‑cients(r2)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 devia‑tions(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 charac‑terized by automated sample pretreatment,and can be applied to the high-throughput rapid screening of odor-causing substances in surface water.

陈秀雯;王磊;柯天英;赵俊明;周铭

上海市环境科学研究院,上海 200233上海市环境科学研究院,上海 200233上海市环境科学研究院,上海 200233上海市环境科学研究院,上海 200233上海市环境科学研究院,上海 200233

化学化工

箭型固相微萃取气相色谱-三重四极杆质谱法异味物质地表水

SPME ArrowGC-MS/MSodor-causing substancessurface water

《分析测试学报》 2026 (5)

980-988,9

上海市2021年度"科技创新行动计划"科学仪器领域项目(21142201300)上海市环境科学研究院创新基金(CX2020180202)

10.12452/j.fxcsxb.25091702

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