固相萃取-超高效液相色谱-串联质谱法同时测定大气降水中9种全氟化合物前体物质  

Simultaneous determination of nine perfluorinated compound precursors in atmospheric precipitation by solid phase extraction and ultra performance liquid chromatography with tandem mass spectrometry

作　　者：张明[1] 唐访良[1] 徐建芬[1] 余波[1] 张伟[1] 姚建良 胡敏华 ZHANG Ming;TANG Fangliang;XU Jianfen;YU Bo;ZHANG Wei;YAO Jianliang;HU Minhua(Hangzhou Environmental Monitoring Central Station,Hangzhou 310007,China;Tonglu Environment Protection Monitoring Station,Hangzhou 311500, China)

机构地区：[1]杭州市环境监测中心站,浙江杭州310007 [2]桐庐县环境保护监测站,浙江杭州311500

出　　处：《色谱》2017年第10期1073-1079,共7页Chinese Journal of Chromatography

基　　金：杭州市社会发展科研攻关项目(20130533B02;20160533B84);杭州市环境保护科技项目(2013HZHB002)~~

摘　　要：采用固相萃取-超高效液相色谱-电喷雾串联三重四极杆质谱联用技术,建立了大气降水中9种全氟化合物前体物质的高通量检测方法。使用HLB固相萃取柱富集和净化降水样品中的目标化合物,以HSS T_3色谱柱(100mm×2.1 mm,1.7μm)为分析柱,甲醇和水作为流动相进行梯度洗脱。质谱以电喷雾负离子电离,采用多反应监测模式检测。9种目标化合物在0.05~5.00μg/L、0.5~50.0μg/L或5.00~500μg/L浓度范围内线性良好,相关系数为0.992 1~0.999 5,方法的检出限为0.05~7.9 ng/L;高、中、低3个添加水平的回收率为76.0%~106%,相对标准偏差为0.72%~13.7%。实验结果表明,该方法灵敏、准确,且具有检测范围广、分析速度快等特点,是一种适用于大气降水样品中全氟化合物前体物质检测分析的方法。A high-throughput detection method has been developed for the determination of nine perfluorinated compound precursors(PFCPs)in atmospheric precipitation by solid phase extraction-ultra performance liquid chromatography coupled with electrospray ionization tan-dem mass spectrometry(SPE-UPLC-ESI-MS/MS).The atmospheric precipitation samples were concentrated and purified with HLB solid phase extraction cartridges.The UPLC separation was performed on an HSS T3column(100mmx2.1mm,1.7pm)utilizing a gradient elution pro-gram of methanol and water as the mobile phases at a flow rate of0.2mL/min.The MS/MS detection was performed under negative electrospray ionization(ESI')in multiple reaction monitoring(MRM)mode.Good linearity was observed in the range of0.05-5.00ug/L,0.50-50.0ug/L or5.00-500ug/L with correlation coefficients from0.9921to0.9995.The limits of detection(LODs)for the nine perfluorinated compound precursors were in the ranges of0.05-7.9ug/L.The recoveries ranged from76.0%to106%with the relative standard deviations between0.72%and13.7%.This method is characterized by high sensitivity and precision,extensive analytical range and quick analytical rate,and can be applied for the analysis of perfluorinated compound precursors in atmospheric precipitation.

关 键 词：固相萃取 超高效液相色谱-电喷雾串联质谱 全氟化合物前体物质 大气降水 

分 类 号：O658[理学—分析化学]