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浙江大学学报(理学版)  2021, Vol. 48 Issue (2): 215-220    DOI: 10.3785/j.issn.1008-9497.2021.02.013
化学     
超临界流体色谱法同时测定海洋水体及沉积物中的4种双酚
干雅平1,2, 楼超艳2, 朱岩2, 甘露3, 陈佳萍3
1.杭州职业技术学院,浙江 杭州 310018
2.浙江大学 化学系,浙江 杭州 310000
3.浙江大学校医院,浙江 杭州 310027
Simultaneous measurement of bisphenols in seawater and marine sediment by supercritical fluid chromatography
GAN Yaping1,2, LOU Chaoyan2, ZHU Yan2, GAN Lu3, CHEN Jiaping3
1.Hangzhou Vocational & Technical College, Hangzhou 310018, China
2.Department of Chemistry, Zhejiang University, Hangzhou 310027, China
3.Zhejiang University Hospital, Zhejiang University, Hangzhou 310027, China
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摘要: 在超临界流体色谱分析条件下,建立了由液液萃取与超临界流体色谱(supercritical fluid chromatography,SFC)同时测定海洋水体中双酚A(BPAF)、双酚AF(BPA)、双酚C(BPC)、四溴双酚A(TBBPA)4种内分泌干扰物的方法。实验结果表明,当SFC流动相为超临界态二氧化碳和甲醇,检测波长为230 nm,柱温为36 ℃、流速为2.0 mL·min-1、系统背压为12 MPa时,5 min内即可实现对双酚类化合物的分离。在线性浓度范围内,双酚类化合物的线性相关系数均高于0.998 9,检出限为0.03~0.06 mg·L-1,4种双酚类化合物在实际样品中的加标回收率为85.7%~112.0%,相对标准偏差均小于10.3%。本文方法可简便快速地检测海洋水体中的双酚,灵敏度和选择性较高,对研究和追踪海洋环境中双酚类化合物的分布具有重要意义。
关键词: 超临界流体色谱海洋水体海洋沉积物双酚内分泌干扰物    
Abstract: An analytical method based on liquid-liquid phase extraction (LLE) coupled with supercritical fluid chromatography (SFC) is proposed for the simultaneous measurement of four bisphenols (bisphenol A,bisphenol AF,bisphenol C and tetrabromobisphenol A) in marine environmental samples. The related parameters of SFC are investigated in this paper.Under the optimum conditions of supercritical CO2 mixed methanol modifier as mobile phase,230 nm as detection wavelength,the 4 bisphenols could be separated completely within 5 minutes (flow rate:2.0 mL·min-1,temperature:36 °C,backpressure:12 MPa). Bisphenols exhibited satisfactory linearity with correlation coefficients higher than 0.998 9.The limits of detection are 0.03-0.06 mg·L-1,respectively. The proposed method was validated by the measurement of 4 bisphenols in marine samples with good spiked recoveries ranged between 85.7% and 112.0% with the relative deviations all were less than 10.3%.This method is convenient,fast,sensitive,accurate and selective,and is of great significance for tracking the distribution of endocrine disrupting compounds in the marine environment.
Key words: supercritical fluid chromatography (SFC)    seawater    marine sediment    bisphenols    endocrine disrupting compounds
收稿日期: 2020-04-02 出版日期: 2021-03-18
CLC:  O  
基金资助: 2019年度高等学校国内访问学者教师专业发展项目(FX2019073);杭州职业技术学院校级科研课题(KY202009);浙江省公益技术研究项目(GC20H0300004);国家自然科学基金资助项目(21974121);浙江省公益技术研究项目(LGC21B070001).
作者简介: 干雅平(1983—),ORCID:http://orcid.org/0000-0001-5776-9580,女,硕士,副教授,主要从事环境污染物分析检测研究,E-mail:122680034@qq.co;
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引用本文:

干雅平, 楼超艳, 朱岩, 甘露, 陈佳萍. 超临界流体色谱法同时测定海洋水体及沉积物中的4种双酚[J]. 浙江大学学报(理学版), 2021, 48(2): 215-220.

GAN Yaping, LOU Chaoyan, ZHU Yan, GAN Lu, CHEN Jiaping. Simultaneous measurement of bisphenols in seawater and marine sediment by supercritical fluid chromatography. Journal of Zhejiang University (Science Edition), 2021, 48(2): 215-220.

链接本文:

https://www.zjujournals.com/sci/CN/10.3785/j.issn.1008-9497.2021.02.013        https://www.zjujournals.com/sci/CN/Y2021/V48/I2/215

1 CESEN M,LENARCIC K,MISLE V,et al.The occurrence and source identification of bisphenol compounds in wastewaters[J].Science of the Total Environment,2018,616-617:744-752. DOI:10. 1016/j.scitotenv.2017.10.252
2 PARMOVA M,HAVLIKOVA L C,CHVOJKA J,et al. An on-line coupling of nanofibrous extraction with column-switching high performance liquid chromatography:A case study on the determination of bisphenol A in environmental water samples[J].Talanta,2018,178:141-146. DOI:10.1016/j.talanta. 2017.08.098
3 张兴宏,黄丽华,戚国荣.三羟基苯甲基氨基均三嗪与双酚A型环氧树脂的固化反应研究[J].浙江大学学报(理学版),2008,35(2):185-190. DOI:10.3785/j.issn.1008-9497.2008.02.015 ZHANG X H,HUANG L H,QI G R.Study on the curing behavior of 2,4,6-tri (hydroxylphenylamine)-s-triazine and diglycidyl ether of bisphenol A[J].Journal of Zhejiang University (Science Edition),2008,35(2):185-190. DOI:10.3785/j.issn.1008-9497.2008.02.015
4 CHUNG S H,DING W H.Isotope-dilution gas chromatography-mass spectrometry coupled with injection-port butylation for the determination of 4-t-octylphenol,4-nonylphenols and bisphenol A in human urine[J].Journal of Pharmaceutical and Biomedical Analysis,2018,149:572-576. 10.1016/j.jpba.2017.11.063
5 TAN X,WAN Y,HUANG Y,et al.Three-dimensional MnO2 porous hollow microspheres for enhanced activity as ozonation catalysts in degradation of bisphenol A[J]. Journal of Hazardous Materials,2017,321:162-172. DOI:10.1016/j.jhazmat.2016. 09.013
6 CHANG H,SHEN X,SHAO B,et al.Sensitive analysis of steroid estrogens and bisphenol A in small volumes of water using isotope-dilution ultra-performance liquid chromatography-tandem mass spectrometry[J].Environmental Pollution,2018,235:881-888. DOI:10.1016/j.envpol.2018.01.003
7 GAO G,CHEN H,ZHU L,et al.Simultaneous determination of bisphenol A and tetrabromobisphenol A in tea using a modified QuEChERS sample preparation method coupled with liquid chromatography-tandem mass spectrometry[J].Analytical Methods,2017,9(48):6769-6776. 10.1039/c7ay02145c
8 ARCE M M,SANLLORENTE S,ORTIZ M C,et al.Easy-to-use procedure to optimize a chromatographic method:Application in the determination of bisphenol-A and phenol in toys by means of liquid chromatography with fluorescence detection[J]. Journal of Chromatography A,2018,1534:93-100. 10.1016/j.chroma.2017.12.049
9 HAO Z,XIAO Y,JIANG L,et al.Simultaneous determination of bisphenol A,bisphenol F,4-nonylphenol,4-n-nonylphenol,and octylphenol in grease-rich food by Carb/PSA solid-phase extraction combined with high-performance liquid chromatography tandem mass spectrometry[J].Food Analytical Methods,2018,11:589-597. DOI:10.1007/s12161-017-1029-5
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