山东科学 ›› 2021, Vol. 34 ›› Issue (3): 71-79.doi: 10.3976/j.issn.1002-4026.2021.03.011

• 环境与生态 • 上一篇    下一篇

固相萃取-高效液相色谱-串联质谱法分析环境水样中5种酚类化合物

刘友彬1,2,李玉阳1,李燕1*   

  1. 1. 济南大学 化学与化工学院,山东 济南 2500122. 山东省化工研究院,山东 济南 250014
  • 收稿日期:2020-09-18 出版日期:2021-06-20 发布日期:2021-06-07
  • 通信作者: 李燕,女,实验师,研究方向为分析化学。Tel:13583199343, E-mail: 10849366591@qq.com
  • 作者简介:刘友彬(1981—),男,学士,工程师,研究方向为化学分析,E-mail:liuyb1122@163.com
  • 基金资助:
    国家青年科学基金(51904114

Determination of five phenolic compounds in environmental water using solid-phase extraction coupled with high-performance liquid chromatography-tandem mass spectrometry

LIU You-bin1,2, LI Yu-yang1, LI Yan1*   

  1. 1. School of Chemistry and Chemical Engineering, University of Jinan, Jinan 250022, China;2.Chemical Technology Academy of Shandong Province, Jinan 250014, China
  • Received:2020-09-18 Online:2021-06-20 Published:2021-06-07

摘要: 结合高效液相色谱-串联质谱法(HPLC-MS/MS),建立了用固相萃取技术富集环境水中5种酚类化合物(双酚F、双酚S、双酚A、辛基酚和壬基酚)的分析方法。样品中目标物经亲油亲水平衡(HLB)固相萃取柱富集,使用二氯甲烷/乙腈梯度洗脱。样品经C18色谱柱分离,采用高效液相色谱-负离子-电喷雾(ESI)串联质谱,多反应监测模式(MRM),外标法定量分析。5种双酚类化合物的线性范围为1~500 ng/L,方法检出限为0.050.15 ng/L,线性相关系数为0.998 70.999 7,精密度在2.54%7.88%,三个水平的回收率在89.40%104.2%,并应用4种不同类型环境水样成功进行分析。该方法可以同时测定环境水样中5种双酚类化合物,方法准确可靠、灵敏度高。

关键词: 固相萃取, 高效液相色谱-串联质谱, 酚类化合物, 环境水

Abstract: In this study, the presence of five phenolic compounds-bisphenol F, bisphenol S, bisphenol A, octyl phenol, and nonyl phenol-in environmental water was determined using solid-phase extraction coupled with high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The compounds were enriched using the hydrophile-lipophile balance column and then eluted using dichloromethane/acetonitrile. The samples were separated using C18 chromatographic column with methanol-water as mobile phase and then detected via HPLC-MS/MS under the multiple-reactions-monitoring mode with the negative-ion mode and quantified using an external standard method. Under optimal conditions, the method exhibits a wide linear response to the five phenolic compounds, ranging 1~500 ng/mL, with a low detection limit of 0.05~0.15 ng/L. The correlation coefficients were between 0.998 7 and 0.999 7. Satisfactory precision (relative standard deviation: 2.54%~7.88%, n=5) and excellent recoveries of 89.40%~104.2% for analytes determination in spiked water samples were observed. The method was successfully applied to four types of environmental water, results show that the proposed method can simultaneously determinate five phenolic compounds in environmental water with high accuracy and sensitivity.

Key words: solid-phase extraction, high-performance liquid chromatography-tandem mass spectrometry, phenolic compounds, environmental water

中图分类号: 

  • O657.34