固相萃取-超高效液相色谱-电喷雾串联质谱法同时测定地表水中16种全氟有机化合物  

Simultaneous determination of sixteen perfluorinated organic compounds in surface water by solid phase extraction and ultra performance liquid chromatography with electrospray ionization tandem mass spectrometry

作　　者：张明[1] 唐访良[1] 俞雅雲 陈峰[1] 徐建芬[1] 叶永根[1] 

机构地区：[1]杭州市环境监测中心站,浙江杭州310007

出　　处：《色谱》2014年第5期472-476,共5页Chinese Journal of Chromatography

基　　金：杭州市社会发展科研攻关项目(20130533B02);杭州市环境保护科技项目(2013HZHB002)

摘　　要：建立了固相萃取-超高效液相色谱-电喷雾串联三重四极杆质谱联用技术分析水中16种全氟有机化合物的高通量检测方法。样品经 WAX 固相萃取柱富集和净化后，采用 Waters ACQUITY UPLCTM BEH C18色谱柱，含2 mmol/L乙酸铵的甲醇和含2 mmol/L乙酸铵的水作为流动相进行梯度洗脱，质谱采用电喷雾负离子电离，多反应监测模式检测。16种全氟有机化合物在0.5~100μg/L或1.0~100μg/L 浓度范围内线性关系良好，相关系数为0.9987~0.9999，方法的检出限为0.06~0.46 ng/L；高、中、低3个添加水平的回收率为67.6％~103％，相对标准偏差为2.94％~12.0％。结果表明，该方法灵敏、准确且检测范围广，分析速度快，是一种适于实际水样中全氟有机化合物检测分析的方法。A high-throughput detection method has been developed for the determination of six-teen perfluorinated organic compounds（ PFCs）in surface water by solid phase extraction-ultra performance liquid chromatography coupled with electrospray ionization tandem mass spec-trometry（ SPE-UPLC-ESI-MS/MS）. The water samples were concentrated and purified through WAX solid phase extraction cartridges. The UPLC separation was performed on an ACQUITY UPLCTM BEH C18 column utilizing a gradient elution program of methanol（containing 2 mmol/L ammonium acetate）and water（ containing 2 mmol/L ammonium acetate）as the mobile phases at a flow rate of 0. 4 mL/min. The MS/MS detection was performed under negative electrospray ionization（ ESI-）in multiple reaction monitoring（ MRM）mode. Good linearities were observed in the range of 0. 5-100 μg/L or 1. 0-100 μg/L with correlation coefficients from 0. 998 7 to 0. 999 9. The limits of detection（ LODs）for the sixteen perfluorinated organic compounds were in the range of 0. 06-0. 46 ng/L. The recoveries ranged from 67. 6% to 103% with the relative standard deviations between 2. 94% and 12. 0%. This method was characterized by high sensitiv-ity and precision,extensive range and high speed,and can be applied for the analysis of PFC contaminants in surface water.

关 键 词：固相萃取 超高效液相色谱 电喷雾串联质谱 全氟有机化合物 地表水 solid phase extraction( SPE) ultra performance liquid chromatography( UPLC) ELECTROSPRAY IONIZATION tandem mass spectrometry( ESI-MS MS) 

分 类 号：O658[理学—分析化学]