顶空固相微萃取/气相色谱-串联质谱法测定环境水中苯系物及氯苯类污染物  

Determination of Benzene Series and Chlorobenzenes Pollutants in Environmental Water by Headspace Solid Phase Microextraction Coupled with Gas Chromatography-Tandem Mass Spectrometry

作　　者：侯新茹 仝凯旋 常巧英[1,3] 张虹艳 陈辉 李相阳[2] 张佳琳 李玲 HOU Xin-ru;TONG Kai-xuan;CHANG Qiao-ying;ZHANG Hong-yan;CHEN Hui;LI Xiang-yang;ZHANG Jia-lin;LI Ling(Chinese Academy of Inspection and Quarantine,Beijing 100176,China;College of Food Science and Engineering,Beijing Agricultural University,Beijing 102206,China;National Center of Technology Innovation for Dairy,Hohhot 010000,China)

机构地区：[1]中国检验检疫科学研究院,北京100176 [2]北京农学院食品科学与工程学院,北京102206 [3]国家乳业技术创新中心,内蒙古呼和浩特010000

出　　处：《分析测试学报》2025年第2期275-284,共10页Journal of Instrumental Analysis

基　　金：国家重点研发计划(2022YFC3700901);国家乳业技术创新中心支持项目(2023-KFKT-28)。

摘　　要：采用顶空固相微萃取结合气相色谱-串联质谱(HS-SPME/GC-MS/MS),建立了一种同时测定水样中8种苯系物和12种氯苯类污染物的方法。采用DB-Heavy-Wax(2.1 mm×50 mm,1.7μm)色谱柱分离,通过对升温程序和质谱条件的优化,对待测物进行色谱分离和特征识别。确定最佳前处理条件:向20 mL顶空瓶中加入10 mL水样及2 g NaCl,在55℃下以500 r/min振荡1 min,萃取时间为10 min,解吸时间为1 min。在最优实验条件下,20种分析物的线性范围为0.000 2~50μg/L,相关系数(r^(2))为0.996 0~0.999 7。方法检出限(LOD)为0.000 1~0.2μg/L,定量下限(LOQ)为0.000 2~0.5μg/L;在不同加标水平(1、2、10倍LOQ)下的回收率分别为75.4%~119%、72.7%~109%和97.8%~118%,日内和日间相对标准偏差(RSD)均不大于19%。采用该法对20批环境水样进行检测,其中1批样品检出甲苯。该方法具有效率高、灵敏度高、自动化程度高、环境友好的优点,可为环境保护和污染物监测提供强有力的技术支持。In this study,the method for the simultaneous determination of eight benzene series(in⁃cluding benzene,toluene,ethylbenzene,o-xylene,p-xylene,m-xylene,cumene and styrene)and 12 chlorobenzenes(CBs)(including chlorobenzene,1,3-dichlorobenzene,1,4-dichloroben⁃zene,1,2-dichlorobenzene,1,3,5-trichlorobenzene,1,2,4-trichlorobenzene,1,2,3-tri⁃chlorobenzene,1,2,3,5-tetrachlorobenzene,1,2,4,5-tetrachlorobenzene,1,2,3,4-tetrachlorobenzene,pentachlorobenzene and hexachlorobenzene)in water samples was established by headspace solid phase microextraction coupled with gas chromatography-tandem mass spectrome⁃try(HS-SPME/GC-MS/MS).The DB-Heavy-Wax(2.1 mm×50 mm,1.7μm)chromatographic col⁃umn was utilized for the separation of complex mixture in water samples.The chromatographic separa⁃tion and feature recognition of the analytes were conducted by fine-tuning the temperature gradient and mass spectrometry parameters to achieve optimal resolution and sensitivity.The optimum pre⁃treatment conditions were set as follows:10 mL water sample and 2 g NaCl were added to a 20 mL headspace bottle,shake for 1 min at 500 r/min at 55℃,the extraction time was 10 min,and the de⁃sorption time was 1 min.Under the optimal experimental conditions,the results showed that the linear ranges of 20 analytes was situated between 0.0002μg/L to 50μg/L.The calibration curves exhib⁃ited high linearity with the correlation coefficient(r2)ranging from 0.9960 to 0.9997.The limits of detection(LODs)for the analytes was located from 0.0001μg/L to 0.2μg/L,and the limits of quan⁃titation(LOQs)was between 0.0002μg/L to 0.5μg/L.Recoveries of the 20 target compounds in water sample were between 75.4% to 119% with the concentration of LOQ,between 72.7%to 109%with the concentration of twice of LOQ,and between 97.8% to 118% with the concentration of 10 times of LOQ.Both the intra-day and the inter-day relative standard deviations(RSDs)were not more than 19%.Consequently,this method was employed to detect 20 batches of environmental water sam�

关 键 词：环境水 顶空固相微萃取 气相色谱-串联质谱 苯系物 氯苯类污染物 

分 类 号：O657.7[理学—分析化学] X132[理学—化学]