柱前衍生-SPE-GC/MS法测定水中痕量溴代苯酚

doi:10.3969/j.issn.1000-1565.2022.04.009

河北大学学报(自然科学版) ›› 2022, Vol. 42 ›› Issue (4): 395-402.DOI: 10.3969/j.issn.1000-1565.2022.04.009

柱前衍生-SPE-GC/MS法测定水中痕量溴代苯酚

葛嘉雨,梁海燕,刘冬,李春灵,张丰泉,赵茜

收稿日期:2021-09-28 出版日期:2022-07-25 发布日期:2022-09-14
通讯作者: 赵茜(1982—)
作者简介:葛嘉雨(1997—),女,河南安阳人,新乡医学院硕士研究生.E-mail:1150559062@qq.com
基金资助:
国家自然科学基金资助项目(21707115);河南省科技攻关项目(212102311076,212102210121);新乡医学院博士科研启动基金资助项目(XYBSKYZZ201518)

Determination of trace bromophenols in water by precolumn derivatization-SPE-GC/MS

GE Jiayu, LIANG Haiyan, LIU Dong, LI Chunling, ZHANG Fengquan, ZHAO Qian

School of Public Health, Xinxiang Medical University, Xinxiang 453003, China

Received:2021-09-28 Online:2022-07-25 Published:2022-09-14

摘要/Abstract

摘要： 采用固相萃取法对水样中的溴酚(BPs)进行富集纯化,以乙酸酐为衍生化试剂,气相色谱-质谱联用仪为检测仪器,建立适于水中痕量BPs的分析方法,并通过以市政供水为测试水样的加标回收实验对该方法进行评价. 在优化后的实验条件下,BPs衍生后具有较好的色谱响应信号和色谱行为,定性检出限为0.8~17.7 ng/mL,空白加标回收率为93.2%~114.5%,以市政供水为水样加标回收率为68.3%~110.1%(其中仅2,4,6-三溴苯酚加标回收率相对较低,为68.3%~73.0%),相对标准偏差均小于20%. 所建立的分析方法灵敏度、回收率和重复性均较好,可以用于实际水样中BPs的测定.

关键词: 溴代苯酚, 柱前衍生, 固相萃取法, 气相色谱-质谱法

Abstract: In this work, bromophenols(BPs)in water samples were enriched by solid phase extraction, with acetic anhydride as derivative reagent and gas chromatography-mass spectrometer as detection instrument and an analysis method suitable for trace BPs in water was established. The method was evaluated by the standard recovery experiment of municipal water sample. After derivatization, BPs showed good chromatographic response signal. The detection limits were 0.8—17.7 ng/mL. The addition recoveries of blank water and municipal water ranged from 93.2% to 114.5%, 68.3% to 110.1%, and only the addition recoveries of 2,4,6-tribromophenol(2,4,6-TBP)was low, ranged from 68.3% to 73.0%. The relative standard deviations were less than 20%. This method was proved to have good sensitivity, recovery and repeatability, and can be applied for the determination of BPs in actual water samples.

Key words: bromophenols, precolumn derivation, solid phase extraction, gas chromatography-mass spectrometry

中图分类号:

O656.31

葛嘉雨,梁海燕,刘冬,李春灵,张丰泉,赵茜. 柱前衍生-SPE-GC/MS法测定水中痕量溴代苯酚[J]. 河北大学学报(自然科学版), 2022, 42(4): 395-402.

GE Jiayu, LIANG Haiyan, LIU Dong, LI Chunling, ZHANG Fengquan, ZHAO Qian. Determination of trace bromophenols in water by precolumn derivatization-SPE-GC/MS[J]. Journal of Hebei University(Natural Science Edition), 2022, 42(4): 395-402.

参考文献

[1] WANG J, HAO Z N, SHI F Q, et al. Characterization of brominated disinfection byproducts formed during the chlorination of aquaculture seawater[J]. Environ Sci Technol, 2018, 52(10): 5662-5670. DOI:10.1021/acs.est.7b05331.
[2] ZHAI H Y, ZHANG X R, ZHU X H, et al. Formation of brominated disinfection byproducts during chloramination of drinking water: new polar species and overall kinetics[J]. Environ Sci Technol, 2014, 48(5): 2579-2588. DOI:10.1021/es4034765.
[3] PAN Y, WANG Y, LI A M, et al. Detection, formation and occurrence of 13 new polar phenolic chlorinated and brominated disinfection byproducts in drinking water[J]. Water Res, 2017, 112: 129-136. DOI:10.1016/j.watres.2017.01.037.
[4] 王莹,陈泽智,李爱民,等.13种新型极性苯酚类氯/溴代消毒副产物的生成机理[J].环境化学, 2017, 36(10): 2089-2099. DOI:10.7524/j.issn.0254-6108.2017021501.
[5] 李欢,李正魁,李爱民,等.新型溴代苯酚类消毒副产物的氯化降解机制[J].环境科学, 2017, 38(8): 3273-3280. DOI:10.13227/j.hjkx.201612221.
[6] 张晓,程婷,陈晨,等.紫外/亚硫酸钠体系对2, 4, 6-三溴酚的脱溴效果及机理[J].无机盐工业, 2020, 52(12): 69-74. DOI:10.11962/1006-4990.2020-0008.
[7] JIANG J, GAO Y, PANG S Y, et al. Oxidation of bromophenols and formation of brominated polymeric products of concern during water treatment with potassium permanganate[J]. Environ Sci Technol, 2014, 48(18): 10850-10858. DOI:10.1021/es5008577.
[8] LIN K D, YAN C, GAN J. Production of hydroxylated polybrominated diphenyl ethers(OH-PBDEs)from bromophenols by manganese dioxide[J]. Environ Sci Technol, 2014, 48(1): 263-271. DOI:10.1021/es403583b.
[9] ARNOLDSSON K, ANDERSSON P L, HAGLUND P. Formation of environmentally relevant brominated dioxins from 2, 4, 6-tribromophenol via bromoperoxidase-catalyzed dimerization[J]. Environ Sci Technol, 2012, 46(13): 7239-7244. DOI:10.1021/es301255e.
[10] 张莘民,杨凯.固相萃取技术在我国环境化学分析中的应用[J].中国环境监测, 2000, 16(6): 53-57. DOI:10.19316/j.issn.1002-6002.2000.06.022.
[11] 高利芳,陈如登,郭辉,等.气相色谱和气相色谱质谱联用在农药残留检测中的应用[J]. 福建农业科技, 2015(8): 73-75. DOI:10.13651/j.cnki.fjnykj.2015.08.029.
[12] 张玺恩,王笛,许风国.化学衍生化技术在靶向代谢组学LC-MS中的应用与进展[J].中国药科大学学报, 2021, 52(1): 31-37. DOI:10.11665/j.issn.1000-5048.20210104.
[13] 蔡灏兢,陈广银,夏飞.柱前衍生化-固相萃取-气相色谱法快速测定水中五氯酚[J].环境监控与预警, 2018, 10(5): 22-25. DOI:10.3969/j.issn.1674-6732.2018.05.005.
[14] 徐继林,严小军,徐年军,等.海产品中溴酚类海洋风味素的气相色谱-质谱联用分析[J].水产学报, 2004, 28(1): 100-105. DOI:10.3321/j.issn: 1000-0615.2004.01.017.
[15] 邱丰艳,韩飞,郑增尧,等.丹酰氯柱前衍生-HPLC荧光法测定食品接触材料中烷基酚类化合物迁移量[J].分析试验室, 2017, 36(10): 1188-1192. DOI:10.13595/j.cnki.issn1000-0720.2017.0255.
[16] 崔君,顾华,张强.改进的五氟苄基溴衍生化反应测定水中酚类化合物[J].分析试验室, 2021, 40(1): 54-58. DOI:10.13595/j.cnki.issn1000-0720.2020.051901.
[17] 李艳平.固相萃取技术在我国环境化学分析中的应用[J].化工设计通讯, 2018, 44(8): 214. DOI:10.3969/j.issn.1003-6490.2018.08.186.
[18] CHI X Y, LIU J Y, YU M, et al. Analysis of bromophenols in various aqueous samples using solid phase extraction followed by HPLC-MS/MS[J]. Talanta, 2017, 164: 57-63. DOI:10.1016/j.talanta.2016.11.010.
[19] YANG K L, ZHANG Y L, DONG Y P, et al. Selectivity of solid phase extraction for dissolved organic matter in the hypersaline Da Qaidam Lake, China[J]. Environ Sci: Processes Impacts, 2017, 19(11): 1374-1386. DOI:10.1039/c7em00263g.
[20] 李利荣,吴宇峰,杨家凤,等.土壤中64种痕量半挥发性有机污染物的分析方法研究[J].分析试验室, 2007, 26(1): 79-84. DOI:10.3969/j.issn.1000-0720.2007.01.019.
[21] 徐英江,张世娟,宫向红,等.凝胶渗透色谱净化-气相色谱-质谱法测定水产品中的溴酚类化合物[J].质谱学报, 2011, 32(6): 350-354, 366.
[22] 郭亚芸,丁燕,胡效亚,等.表面活性剂辅助-凝固-漂浮分散液液微萃取/高效液相色谱法测定环境水样中酚类化合物[J].分析测试学报, 2015, 34(9): 1040-1044. DOI:10.3969/j.issn.1004-4957.2015.09.010. (

柱前衍生-SPE-GC/MS法测定水中痕量溴代苯酚

Determination of trace bromophenols in water by precolumn derivatization-SPE-GC/MS

PDF (PC)

可视化

摘要/Abstract

引用本文

使用本文

参考文献

相关文章 1

编辑推荐

Metrics

本文评价