摘要
本研究建立了固相萃取结合高效液相色谱-串联质谱测定水体中痕量三苯乙烯基苯酚聚氧乙烯醚(TSPEOn,n=6—29)的方法.水样经HLB柱富集,用10 mL二氯甲烷-甲醇混合溶液(1∶1)洗脱,将洗脱液氮吹至近干后,用乙腈定容至0.5 mL.采用C18(2.1 mm×50 mm,5μm)+Silica(2.1 mm×150 mm,4μm)串联色谱柱,以乙腈和2 mmol·L-1乙酸铵水为流动相,在电喷雾正离子、多反应监测模式下对TSPEOs进行定性分析,外标法进行定量分析.结果表明,TSPEOn(n=6—29)在0.06—512.5μg·L-1浓度范围内线性关系良好,线性相关系数在0.989—0.999之间,方法检出限为0.001—0.22 ng·L-1,定量限为0.004—0.72 ng·L-1,平均回收率在67.4%—103.3%之间,相对标准偏差为0.7%—14.8%,该方法可用于实际地表水样中痕量TSPEOn(n=6—29)的测定.
In this work,we developed a new method based on solid phase extraction-high performance liquid chromatography coupled with tandem mass spectrometry for analysis of trace tristyrylphenol ethoxylates(TSPEOn,n=6—29)in water.The water sample was concentrated by passing it through a HLB solid phase extraction cartridge.The HLB cartridge was eluted using 10 mL of a mixed solution of dichloromethane and methanol(1∶1).The eluent was then concentrated under high-purity nitrogen,and reconstituted with acetonitrile to 0.5 mL for analysis.The separation was performed on a C18 column(2.1 mm×50 mm,5μm)and a Silica column(2.1 mm×150 mm,4μm)with a mobile phase of acetonitrile and 2 mmol·L-1 ammonium acetate aqueous solution.The TSPEOs were determined using electrospray ionization source in positive ion mode with multiple reaction monitoring.The external standard method was used for quantification.The results showed that TSPEOn(n=6—29)showed good linearity in the concentration range of 0.06—512.5μg·L-1 with correlation coefficients of 0.989—0.999.The limits of detection were 0.001—0.22 ng·L-1,and the limits of quantification were 0.004—0.72 ng·L-1.The average recoveries of TSPEOn(n=6—29)were ranged from 67.4%to 103.3%with the relative standard deviations of 0.7%—14.8%.This method could be applied to determine trace TSPEOn(n=6—29)in surface water.
作者
张雅莉
高俊敏
李春梅
周杰
贺青华
王静
金芬
ZHANG Yali;GAO Junmin;LI Chunmei;ZHOU Jie;HE Qinghua;WANG Jing;JIN Fen(Key Laboratory of the Three Gorges Reservoir Region's Eco-Environment,Ministry of Education,Chongqing University,Chongqing,400045,China;Key Laboratory of Agro-Product Quality and Safety,Institute of Quality Standard and Testing Technology for Agro-Products,Chinese Academy of Agricultural Sciences,Beijing,100081,China)
出处
《环境化学》
CAS
CSCD
北大核心
2020年第7期1941-1948,共8页
Environmental Chemistry
基金
中央级公益性科研院所基本科研业务费专项(Y2017PT37)
中国农业科学院“科研英才培育工程”项目
中国农业科学院创新工程项目
国家自然科学基金(21976021)资助
关键词
三苯乙烯基苯酚聚氧乙烯醚
水体
固相萃取
高效液相色谱-串联质谱
tristyrylphenol ethoxylates
water
solid phase extraction
high performance liquid chromatography-tandem mass spectrometry
