手搖輔助超音波增強乳化液液微萃取分析水樣中的內分泌干擾酚類

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手搖輔助超音波增強乳化液液微萃取分析水樣中的內分泌干擾酚類

Analysis of endocrine-disrupting phenols in water samples by shake-assisted ultrasound-enhanced emulsification liquid-liquid microextraction

舒明威 , Masters　　Advisor：黃賢達　　

繁體中文

液相微萃取；樣品前濃縮；極致效能液相層析儀；內分泌干擾酚類； 4-第三丁基苯酚； 4-肉桂苯酚； 4-第三辛基苯酚； 2,4-雙丁基苯酚；壬基苯酚；烷基苯酚；環境荷爾蒙； Liquid phase mictoextraction ； Sample preconcentration ； Ultra performance liquid chromatography (UPLC) ； Endocrine-disrupting phenols ； 4-tert-butylphenol ； 4-cumylphenol ； 4-tert-octylphenol ； 2,4-di-tert-butylphenol ； 4-nonylphenol ； Alkylphenol ； Environmental hormone

Abstract │ Reference (74) │ Altmetrics

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A simple and fast equilibrium liquid-phase microextraction method based on shake-assisted ultrasound-enhanced emulsification liquid-liquid microextraction (SAUELLME) technique combined with ultra performance liquid chromatography (UPLC) with UV detection was developed for the preconcentration and determination of five endocrine-disrupting phenols (EDPs) in seawater samples and detergent samples. The EDPs studied were 4-tert-butylphenol (4-t-BP), 4-cumylphenol (4-CP), 4-tert-octylphenol (4-t-OP), 2,4-di-tert-butylphenol (2,4-di-t-BP) and 4-nonylphenol (4-NP). For SAUELLME, dispersion of the fine droplets of a low density organic extraction solvent into the aqueous sample is formed by use of the first step shake- assisted for mixing, and then the fine droplets could extract target analytes toward equilibrium faster because of the shorter diffusion distance and larger surface area by ultrasound-enhanced emulsification.
Different experimental parameters were controlled and the optimum conditions found were: 25 μL of 1-bromohexadecane as the extraction solvent, 5 ml water samples, 1 minute ultrasound extraction time, 10 seconds shake-assisted time, centrifugation for 3 min at 5000 rpm, 1g NaCl for ionic strength, no pH adjustment, centrifugation tube was lying on the center of ultrasonic bath system.
The correlation coefficient (γ2 ) greater than 0.995 for calibration curve range. The limit of detection (LOD) was 0.5 to 2.8 ngmL-1, the limit of quantitation (LOQ) was 1.8 to 9.3 ngmL-1 and the relative standard deviation (RSD) ranged from 4.2 % to 10.3 % for seawater samples. The limit of detection (LOD) was 0.4 to 2.4 μgmL-1, the limit of quantitation (LOQ) was 1.6 to 8.2 μgmL-1 and the relative standard deviation (RSD) ranged from 4.7 % to 10.0 % for detergent samples.
Applying proposed method to spiked seawater samples and detergent samples in order to determine matrix effects. The relative recovery was 96 % to 109 % for seawater samples and 81 % to 106 % for detergent samples.

Reference ( 74 ) 〈TOP〉

荷爾蒙物質管理及環境流布調查”，行政院環境保護署環境檢驗所
連結：
[5] J.-P. Myers, T. Colborn, D. Dumanoski, （1996）Our Stolen Future,
連結：
[8] 林維雋，“以一維及二維氣相層析質譜儀檢測生物檢體中烷基酚之分析與研究”，2007，國立中央大學化學研究所碩士論文
連結：
[12] 特殊健康危害專題季刊，發行單位：行政院衛生署國民健康局；編輯單位：國立成功大學，2010
連結：
[13] T. Shioda, M. Wakabayashi, Chemosphere, 40 (2000) 39-43
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