Arid
DOI10.1016/j.chroma.2004.06.121
Determination of weakly acidic endocrine-disrupting compounds by liquid chromatography-mass spectrometry with post-column base addition
Carabias-Martinez, R; Rodriguez-Gonzalo, E; Revilla-Ruiz, P
通讯作者Carabias-Martinez, R
会议名称8th International Symposium on Hyphenated Techniques in Chromatography and Hyphenated Chromatographic Analyzers (HTC-8)
会议日期FEB 04-06, 2004
会议地点Brugge, BELGIUM
英文摘要

A sensitive analytical method based on liquid chromatography-electrospray ionisation mass spectrometry (LC-ESI-MS) has been developed for the determination of seven endocrine-disrupting compounds: 4-n-nonylphenol (NP), 4-tert-butylphenol (t-BP), bisphenol A (BPA), 2,4-dichlorophenol (DCP), 2,4,5-trichlorophenol (TCP), pentachlorophenol (PCP) and 4-tert-butylbenzoic acid (BBA) in water samples. To achieve a good LC separation, acidification of the LC mobile phase was necessary, but this led to MS signal suppression for the less acidic compounds. In order to enhance the sensitivity for these analytes, post-column addition of different bases such as ammonia, trimethylamine, and 1,8-diazabicyclo-(5,4,0)undec-7-en (DBU) was evaluated. The post-column addition of base is proposed here to raise effluent pH, helping in the ionisation process of the compounds with higher pK(a) values (t-BP, BPA, DCP and NP). The use of DBU, diluted in MeOH, proved to be the most efficient post-column reagent for enhancing the NIS signal. The signal-to-noise ratios for t-BP and NP increased by more than 200-fold and 35-fold, respectively, whereas for DCP and BPA an increase of about 10-fold was achieved. This strategy permitted direct determination of the seven compounds at low ppb levels. For application to real water samples, an extraction and preconcentration step using the solid-phase extraction (SPE) technique was carried out. The applicability of three solid-phase materials-Bond Elut C-18, and two polymeric sorbents: LiChrolut EN and Oasis HLB-and the optimization of other SPE parameters such as the elution solvent and sample volume used, were studied in order to maximize extraction efficiency. Oasis HLB provided the best results, obtaining-with the proposed SPE procedure-satisfactory percentage recoveries for all compounds (70-110%) with the exception of NP, for which a recovery of 54% was achieved. Application of the whole method, SPE-LC-(ESI)-MS, to natural waters permitted low nanogram-per-liter determination of all seven compounds. (C) 2004 Elsevier B.V. All rights reserved.


英文关键词water analysis post-column base addition solid-phase extraction endocrine disruptors diazabicyclo-(5,4,0)undec-7-en
来源出版物JOURNAL OF CHROMATOGRAPHY A
ISSN0021-9673
EISSN1873-3778
出版年2004
卷号1056
期号1-2
页码131-138
出版者ELSEVIER SCIENCE BV
类型Article;Proceedings Paper
语种英语
国家Spain
收录类别SCI-E ; CPCI-S
WOS记录号WOS:000225143800018
WOS关键词SOLID-PHASE EXTRACTION ; ENVIRONMENTAL WATER SAMPLES ; BISPHENOL-A ; TRANSFORMATION PRODUCTS ; GAS-CHROMATOGRAPHY ; HERBICIDES ; CHEMICALS ; PHENOLS ; XENOESTROGENS ; PESTICIDES
WOS类目Biochemical Research Methods ; Chemistry, Analytical
WOS研究方向Biochemistry & Molecular Biology ; Chemistry
资源类型会议论文
条目标识符http://119.78.100.177/qdio/handle/2XILL650/294996
作者单位(1)Univ Salamanca, Fac Quim, Dept Quim Analit Nutr & Bromatol, E-37008 Salamanca, Spain
推荐引用方式
GB/T 7714
Carabias-Martinez, R,Rodriguez-Gonzalo, E,Revilla-Ruiz, P. Determination of weakly acidic endocrine-disrupting compounds by liquid chromatography-mass spectrometry with post-column base addition[C]:ELSEVIER SCIENCE BV,2004:131-138.
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