固相微萃取-气相色谱/质谱联用技术测定水样中13种有机磷酸酯  

Determination of Thirteen Organophosphate Esters in Water Samples Using Solid-phase Microextraction Coupled with Gas Chromatography-Mass Spectrometry

作　　者：罗庆 王诗雨 单岳 孙丽娜 王辉 LUO Qing;WANG Shi-yu;YUE Shan;SUN Li-na;WANG Hui(Key Laboratory of Regional Environment and Eco-Remediation of Ministry of Education, College of Environment,Shenyang University,Shenyang 110044)

机构地区：[1]沈阳大学环境学院区域污染环境生态修复教育部重点实验室,辽宁沈阳110044

出　　处：《分析科学学报》2018年第6期751-756,共6页Journal of Analytical Science

基　　金：辽宁省自然科学基金重点项目(No.20170520384);国家重点基础研究发展计划(No.2014CB441100)

摘　　要：建立了固相微萃取-气相色谱/质谱联用技术检测水中13种有机磷酸酯阻燃剂/增塑剂的分析方法。选取PDMS-DVB涂层纤维作为固相微萃取的萃取纤维,并对样品溶液的pH值、离子强度、助溶剂、萃取时间、萃取温度、搅拌速度等主要参数进行了优化。结果表明,最佳萃取条件为:水样pH值调整为4,加入25%的NaCl和5%的乙腈,然后在40℃下以600r/min搅拌萃取50min。方法具有较宽的线性范围,相关系数大于0.9927,方法的检出限为1.1～27.3ng/L,定量限为3.7～90.1ng/L,实际水样的加标回收率为68.2%～90.3%,相对标准偏差小于15%。该方法简便、快速、准确,可用于水体中13种有机磷酸酯的测定。A reliable and convenient solid-phase microextraction method combined with gas chromatography-ion trap tandem mass spectrometry for the simultaneous determination of thirteen organophosphate esters in water samples was developed.The PDMS-DVB fiber was selected as the extraction fiber,and the key extraction parameters influencing extraction efficiency,including pH,salt concentration,co-solvent,extraction time and temperature,and agitation speed were investigated.The optimized extraction conditions were water samples pH=4,containing 25% NaCl and 5%acetonitrile,and agitation at 40℃for 50 min with speed of600 r/min.This method has a wide linear renge,and the correlation coefficients were larger than 0.9927.The detection limits and quantitation limits ranged from 1.1 ng/L to 27.3 ng/L and from 3.7 ng/L to90.1 ng/L,respectively.The recoveries in actual water sample were in the range of 68.2%-90.3%,and the relative standard deviations were less than 15%.The method is simple,rapid and accurate,and colud be used for the determination of 13 organophosphate esters in water samples.

关 键 词：有机磷酸酯 固相微萃取 气相色谱-质谱 水样 

分 类 号：O657.63[理学—分析化学]