摘要
建立了悬浮固化-分散液液微萃取结合液相色谱-串联质谱测定纺织废水中5种痕量磷系阻燃剂的方法。通过对萃取过程中萃取剂、分散剂的种类与体积、盐浓度、溶液pH值等对萃取效率的影响因素优化,确立了最佳萃取条件。采用了密度小于水的十一烷醇(400μL)为萃取剂,甲醇(300μL)为分散剂,控制溶液pH值在6~9之间,NaCl添加量为2 g,萃取时间为涡旋2 min。在优化的萃取条件下,该方法在2~100μg/L均有良好的线性关系,相关系数大于0.995,除二(2,3-二溴丙基)磷酸酯(BIS)的检出限为5μg/L外,三(2-氯乙基)磷酸酯(TCEP)、三(1,3-二氯-异丙基)磷酸酯(TDCP)、三(1-氮丙啶基)氧化膦(TEPA)和三(2,3-二溴丙基)磷酸酯(TRIS)的检出限均为2μg/L。后整理、染色和印花等实际废水样品加标试验表明,方法的平均回收率为71.6%~114.5%,RSD为2.7%~11.2%(n=6)。对11个样品进行检测,其中3个废水样品检出TCEP与TDCP化合物,含量为2.6~3.4μg/L。本方法简单,快速,灵敏度好且环保绿色,能够对纺织废水中的5种痕量磷系阻燃剂进行准确的定性与定量检测。
A rapid method for the determination of five organophosphorus flame retardants(OPFRs)in textile wastewater was established by dispersive liquid-liquid microextraction(DLLME)based on solidification of floating organic drop(SFO)coupled with ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The analytes were extracted from the water samples by SFO-DLLME,which was performed using a mixture of an extraction solvent that was less dense than water,1-undecanol,and a dispersive solvent,methanol.The influences of the SFO-DLLME parameters on the extraction efficiencies were studied.1-Undecanol(extraction solvent,400μL)and methanol(dispersive solvent,300μL)were added to textile wastewater(containing 2 g NaCl)with pH between 6 and 9,and the solution was shaken for 2 min.Under optimum conditions,the linear ranges of the proposed method were from 2μg/L to 100μg/L with correlation coefficients(R2)above 0.99 for all the analytes.The limits of detection(S/N=3)ranged from 2μg/L to 5μg/L.The precision of the method was evaluated in terms of repeatability;the relative standard deviations varied from 2.7%to 11.2%(n=6).The relative recoveries ranged from 71.6%to 117.6%for all analytes.Only 3 of the 11 selected samples were tested positive for OPFRs,and the total concentrations of OPFRs in them were in the range of 2.6-3.4μg/L.Hence,this method is accurate,environmentally friendly,fast,and convenient for the routine analysis of OPFRs in textile wastewater.
作者
何静
叶曦雯
汤志旭
牛增元
罗忻
邹立
HE Jing;YE Xiwen;TANG Zhixu;NIU Zengyuan;LUO Xin;ZOU Li(College of Environmental Science and Engineering, Ocean University of China, Qingdao 266100, China;Qingdao Customs Technology Center, Qingdao 266003, China)
出处
《色谱》
CAS
CSCD
北大核心
2020年第6期679-686,共8页
Chinese Journal of Chromatography
基金
国家重点研发计划(NQI 2016YFF0203702).
关键词
悬浮固化
分散液液微萃取
超高效液相色谱-串联质谱
磷系阻燃剂
纺织废水
solidification of floating organic drop(SFO)
dispersive liquid-liquid microextraction(DLLME)
ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)
organophosphorus flame retardants(OPFRs)
textile wastewater
作者简介
通讯作者:叶曦雯,Tel:(0532)88968060,E-mail:ye.xiwen@163.com;通讯作者:牛增元,Tel:(0532)58653540,E-mail:zyniuqd@163.com.
