采用超高压液相色谱法和一种新的手动增强摇震、超声辅助乳状液微萃取方法，基于漂浮有机液滴的固化作用来测定硝基酚。
Determination of nitrophenols using ultrahigh pressure liquid chromatography and a new manual shaking-enhanced, ultrasound-assisted emulsification microextraction method based on solidification of a floating organic droplet.
机构信息
Department of Chemistry, National Tsing Hua University, Hsinchu 30013, Taiwan.
出版信息
J Chromatogr A. 2012 Jul 13;1246:55-61. doi: 10.1016/j.chroma.2012.02.025. Epub 2012 Feb 16.
Nitrophenols are toxic compounds in the wastewater. In the proposed method, a new technique using a manual shaking-enhanced, ultrasound-assisted emulsification microextraction (MS-USAEME) method based on solidification of a floating organic droplet combined with ultrahigh pressure liquid chromatography (UHPLC) has been developed for the extraction and determination of nitrophenols in aqueous samples. In this method, the low toxicity extraction solvent 1-undecanol was used to extract the nitrophenols. After centrifugation, ice bath was used to solidify the floating extraction solvent, using microtubes to collect the floated extraction solvent and diluting with 30 μL of dimethyl sulfoxide, then injecting into the UHPLC for further analysis. The relative standard deviations (RSD) were 6-12%, enrichment factors (EFs) were 62-500, the relative recoveries (RR) of this method were 80-110% for spiked lake water samples. The detection limits of this method were 0.5-3.0 μg L⁻¹ for spiked lake water and 0.6-3.2 μg L⁻¹ for spiked agriculture water. The further performance of the proposed method was gauged by analyzing field samples.
硝基酚是废水中的有毒化合物。在提出的方法中，开发了一种新的技术，使用手动摇动增强、超声辅助乳化微萃取（MS-USAEME）方法，基于固 定化浮油滴与超高效液相色谱（UHPLC）相结合，用于从水样中提取和测定硝基酚。在该方法中，使用低毒性萃取溶剂 1-十一醇来萃取硝基酚。离心后，使用冰浴将浮 动萃取溶剂固化，使用微量离心管收集浮 动萃取溶剂并用 30 μL 二甲基亚砜稀释，然后注入 UHPLC 进行进一步分析。相对标准偏差（RSD）为 6-12%，富集因子（EF）为 62-500，该方法对加标湖水样品的相对回收率（RR）为 80-110%。该方法对加标湖水的检出限为 0.5-3.0 μg L⁻¹，对加标农业水的检出限为 0.6-3.2 μg L⁻¹。通过分析现场样品进一步评估了该方法的性能。
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