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

HOU Xin-ru; TONG Kai-xuan; CHANG Qiao-ying; ZHANG Hong-yan; CHEN Hui; LI Xiang-yang; ZHANG Jia-lin; LI Ling

doi:10.12452/j.fxcsxb.240607113

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

Scientific Papers | 更新时间：2025-02-12

- Determination of Benzene Series and Chlorobenzenes Pollutants in Environmental Water by Headspace Solid Phase Microextraction Coupled with Gas Chromatography-Tandem Mass Spectrometry
- Journal of Instrumental Analysis Vol. 44, Issue 2, Pages: 275-284(2025)
- 作者机构：
  
  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
- 作者简介：
- 基金信息：
- DOI：10.12452/j.fxcsxb.240607113
  CLC： O657.7;X132
- Published：15 February 2025，
  
  Received：07 June 2024，
  
  Revised：26 August 2024，
  
  Accepted：2024-09-04
- 稿件说明：
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侯新茹,仝凯旋,常巧英,张虹艳,陈辉,李相阳,张佳琳,李玲.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[J].分析测试学报,2025,44(02):275-284.

HOU Xin-ru,TONG Kai-xuan,CHANG Qiao-ying,ZHANG Hong-yan,CHEN Hui,LI Xiang-yang,ZHANG Jia-lin,LI Ling.Determination of Benzene Series and Chlorobenzenes Pollutants in Environmental Water by Headspace Solid Phase Microextraction Coupled with Gas Chromatography-Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2025,44(02):275-284.
侯新茹,仝凯旋,常巧英,张虹艳,陈辉,李相阳,张佳琳,李玲.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[J].分析测试学报,2025,44(02):275-284. DOI： 10.12452/j.fxcsxb.240607113.

HOU Xin-ru,TONG Kai-xuan,CHANG Qiao-ying,ZHANG Hong-yan,CHEN Hui,LI Xiang-yang,ZHANG Jia-lin,LI Ling.Determination of Benzene Series and Chlorobenzenes Pollutants in Environmental Water by Headspace Solid Phase Microextraction Coupled with Gas Chromatography-Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2025,44(02):275-284. DOI： 10.12452/j.fxcsxb.240607113.

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，1.7 μm）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 2~50 μg/L，相关系数（

）为0.996 0~0.999 7。方法检出限（LOD）为0.000 1~0.2 μg/L，定量下限（LOQ）为0.000 2~0.5 μg/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。

Abstract

In this study，the method for the simultaneous determination of eight benzene series（including benzene，toluene，ethylbenzene，

-xylene，

-xylene，cumene and styrene） and 12 chlorobenzenes（CBs）（including chlorobenzene，1，3-dichlorobenzene，1，4-dichlorobenzene，1，2-dichlorobenzene，1，3，5-trichlorobenzene，1，2，4-trichlorobenzene，1，2，3-trichlorobenzene，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 spectrometry（HS-SPME/GC-MS/MS）. The DB-Heavy-Wax（2.1 mm×50 mm，1.7 μm） chromatographic column was utilized for the separation of complex mixture in water samples. The chromatographic separation and feature recognition of the analytes were conducted by fine-tuning t

he temperature gradient and mass spectrometry parameters to achieve optimal resolution and sensitivity. The optimum pretreatment 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 desorption time was 1 min. Under the optimal experimental conditions，the results showed that the linear ranges of 20 analytes was situated between

0.000 2 μg/L to 50 μg/L. The calibration curves exhibited high linearity with the correlation coefficient（

） ranging from 0.996 0 to 0.999 7. The limits of detection（LODs） for the analytes was located from 0.000 1 μg/L to 0.2 μg/L，and the limits of quantitation（LOQs） was between 0.000 2 μg/L to 0.5 μg/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 samples to determine benzene series and chlorobenzene pollutants. As a result，the toluene was successfully detected in one batch of samples，which indicated that this method could effectively meet the analysis requirements of benzene series and chlorobenzene pollutants in environmental water samples. It was considered that this method had several distinct advantages，including high efficiency，high sensitivity，high degree of automation and environmental friendliness（without the use of extractant）. The analytical methods developed in this study could not only provide strong technical support for environmental protection but also play a critical role for pollutant monitoring.

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

Keywords

environmental waterheadspace solid phase microextractiongas chromatography-tandem mass spectrometrybenzene serieschlorobenzenes

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