顶空液相微萃取在环境水样中邻硝基苯酚的萃取机制研究.pdfVIP

.. ... .. 中国药物与临床2012年2月第l2卷第2期Chinese R mediesClinits,Febinary 2012，v01．12，No．2 顶空液相微萃取在环境水样中 邻硝基苯酚的萃取机制研究 陈 璇 白小红 赵凌雁 朱 颖 【摘 要】 目的 探讨顶空液相微萃取在挥发性组分邻硝基苯酚萃取中的萃取机制，建立水样中邻硝基 苯酚的顶空液相微萃取一高效液相色谱测定方法。方法 将密封玻璃瓶中的样品溶液置于恒温磁力搅拌器上搅 拌加热，以甲醇为萃取溶剂将其悬于样品溶液的上部空间，萃取40 s，连续萃取5次，合并萃取液进行高效液相 色谱紫外检测。结果 实验考察了萃取条件对萃取效率的影响；讨论了顶空液相微萃取理论富集倍数、表观富集 倍数和萃取率的公式；阐明了醇类有机溶剂的理化性质与萃取效率之间的相关关系，并对同类醇溶剂的萃取效 率进行了预测；在优化的实验条件下，建立了水样中邻硝基苯酚含量测定方法，线性范围为0．OOOO4～25~g／ml(r= 0．9993，n=15)，检测限为10 pg／ml，方法的相对标准偏差为4．O％～10．1％，平均回收率97．2％一113．3％，富集倍数为 20倍。结论 该方法操作简单、快捷、灵敏度高，对环境样品中挥发性或半挥发性痕量成分的分析具有重要意 义。 【关键词】色谱法，高压液相；邻硝基苯酚；富集倍数；醇溶剂理化性质；萃取效率 Headspace liquid-phase micro-·extraction for ortho-nitrophenol in environmental water sample：a mechanistic study CHEN Xuan,BAl Xiao—hong,ZHA0 Ling-yah,ZHU Ying．Department ofDrugAnalysis．Shanxi Medical U- niversity College ofPharmacy,Taiyuan 030001，China 【Abstract】Objectlve To investigate the mechanisms of headspaee liquid-phase micro—extraction(HS-LPME) for ortho-nitrophenol， a volatile component，and to develop a novel approach for determining the contents in water sample vht HS-LPME coupled with high performance liquid chromatography rHPLC)．Methods The sample solution was contained in a sealed vial，and placed on a thermostatic magnetic agitator for heating and stirring．Five continuous 40．second cycles of extraction was performed using metl1anol as the extractant suspended over the sample solution． Extracts yielded in each cycle were pooled and subiected to HPLC．uhraviolet detection．Results The conditions af- fecting HS．LPME emciency． explore the formulae for theoretical enrichment factor． apparent enrichment factor and extraction efficiency were inv