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采用分散液液微萃取-气相色谱-质谱联用技术测定瓶装水中的邻苯二甲酸酯。

Determination of phthalate esters in bottled water using dispersive liquid–liquid microextraction coupled with GC-MS.

机构信息

Department of Chemistry, King Fahd University of Petroleum and Minerals, Dhahran, Saudi Arabia.

出版信息

J Sep Sci. 2013 Jun;36(12):2003-9. doi: 10.1002/jssc.201300163.

Abstract

Dispersive liquid-liquid microextraction method was developed for the determination of the amount of phthalate esters in bottled drinking water samples and dispersive liquid-liquid microextraction samples were analyzed by GC-MS. Various experimental conditions influencing the extraction were optimized. Under the optimized conditions, very good linearity was observed for all analytes in a range between 0.05 and 150 μg/L with coefficient of determination (R²) between 0.995 and 0.999. The LODs based on S/N = 3 were 0.005-0.22 μg/L. The reproducibility of dispersive liquid-liquid microextraction was evaluated. The RSDs were 1.3-5.2% (n = 3). The concentrations of phthalates were determined in bottled samples available in half shell. To understand the leaching profile of these phthalates from bottled water, bottles were exposed to direct sunlight during summer (temperature from 34-57°C) and sampled at different intervals. Result showed that the proposed dispersive liquid-liquid microextraction is suitable for rapid determination of phthalates in bottled water and di-n-butyl, butyl benzyl, and bis-2-ethylhexyl phthalate compounds leaching from bottles up to 36 h. Thereafter, degradation of phthalates was observed.

摘要

分散液相微萃取法被开发用于测定瓶装饮用水样品中邻苯二甲酸酯的含量,并用 GC-MS 对分散液相微萃取样品进行分析。优化了影响萃取的各种实验条件。在优化的条件下,所有分析物在 0.05 至 150 μg/L 的范围内均表现出非常好的线性,相关系数 (R²) 在 0.995 至 0.999 之间。基于 S/N = 3 的检出限为 0.005-0.22 μg/L。评估了分散液相微萃取的重现性。RSD 为 1.3-5.2%(n = 3)。在半壳装的瓶装样品中测定了邻苯二甲酸盐的浓度。为了了解这些邻苯二甲酸盐从瓶装水中的浸出情况,在夏季(温度为 34-57°C)将瓶子暴露在阳光下,并在不同时间间隔进行采样。结果表明,所提出的分散液相微萃取适用于快速测定瓶装水中的邻苯二甲酸盐以及从瓶子中浸出的二正丁基、丁基苄基和双(2-乙基己基)邻苯二甲酸酯化合物,长达 36 小时。此后,观察到邻苯二甲酸盐的降解。

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