摘要
建立了顶空固相微萃取-气相色谱-三重四极杆质谱法(HS-SPME-GC-MS/MS)测定饮用水中8种卤代苯乙腈(HPANs)的方法,10 mL水样经全自动固相微萃取,热解析进样,Rtx-5型气相色谱柱分离,质谱多反应监测(MRM)测定,外标法定量。结果表明,50/30μm二乙烯苯/活性炭/聚二甲基硅氧烷(DVB/CAR/PDMS)固相微萃取纤维的萃取效果最佳;在10 mL水样中加入4 g NaCl可增加基质的离子强度;HPANs溶液的基质效应为0.79~0.86,基质抑制影响较小,故选用超纯水作为标准曲线的溶剂。8种HPANs具有良好的线性关系,相关系数均>0.998,检出限为0.2~2.0 ng/L,定量限为0.6~5.0 ng/L。3个浓度水平的加标回收率为88.6%~103.6%,相对标准偏差为4.9%~8.8%。在20件出厂水和10件末梢水样品中均未检出8种HPANs。该方法可作为饮用水中HPANs类新型消毒副产物的检测方法。
A method was established for the determination of eight halogenated phenylacetonitriles(HPANs)in drinking water using headspace solid phase microextraction and gas chromatography-triple quadrupole mass spectrometry(HS-SPME-CC-MS/MS).A 10 mL of water sample was subjected to fully automated solid-phase microextraction,thermal analysis injection,Rtx-5 gas chromatography column separation,mass spectrometry multiple reaction monitoring(MRM)determination,and external standard quantification.The results showed that the extraction efficiency of 50/30μm divinylbenzene/activated carbon/polydimethylsiloxane(DVB/CAR/PDMS)solid-phase microextraction fibers was the best.Adding 4 g NaCl to 10 mL of water sample can increase the ionic strength of the matrix;the matrix effect of HPAN aqueous solution was 0.79-0.86,and the matrix inhibition effect was relatively small.Therefore,ultrapure water was selected as the solvent for the standard curve.Eight HPANs have good linear relationships,with correlation coefficients>0.998,detection limits of 0.2-2.0 ng/L,and quantification limits of 0.6-5.0 ng/L.The spiked recovery rates at three levels were 88.6%-103.6%,and the relative standard deviations were 4.9%-8.8%.None of the 8 HPANs were detected in the 20 treated water and 10 peripheral water samples.This method can be used to detect novel HPANs disinfection by products in drinking water.
作者
李浩然
韩志宇
张永
陶晶
詹未
LI Haoran;HAN Zhiyu;ZHANG Yong;TAO Jing;ZHAN Wei(Beijing Center for Disease Prevention and Control,Beijing 100013,China)
出处
《分析试验室》
北大核心
2025年第9期1412-1416,共5页
Chinese Journal of Analysis Laboratory
关键词
饮用水
消毒副产物
卤代苯乙腈
固相微萃取
drinking water
disinfection byproducts
halogenated-phenylacetonitriles
solid-phase microextraction
