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

doi:10.3724/SP.J.1123.2017.06025

色谱 ›› 2017, Vol. 35 ›› Issue (10): 1073-1079.DOI: 10.3724/SP.J.1123.2017.06025

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

张明¹, 唐访良¹, 徐建芬¹, 余波¹, 张伟¹, 姚建良², 胡敏华²

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

收稿日期:2017-06-27 出版日期:2017-10-08 发布日期:2017-10-18
通讯作者: 唐访良,E-mail:TangFL001@163.com.
基金资助:
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）.

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

ZHANG Ming¹, TANG Fangliang¹, XU Jianfen¹, YU Bo¹, ZHANG Wei¹, YAO Jianliang², HU Minhua²

1. Hangzhou Environmental Monitoring Central Station, Hangzhou 310007, China;
2. Tonglu Environment Protection Monitoring Station, Hangzhou 311500, China

Received:2017-06-27 Online:2017-10-08 Published:2017-10-18
Supported by:
Scientific Research Fund for the Social Development of Hangzhou (Nos. 20130533B02, 20160533B84); Research Fund for the Environmental Protection of Hangzhou (No. 2013HZHB002).

摘要/Abstract

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 T₃色谱柱（100 mm×2.1 mm， 1.7 μm）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0.05~5.00 μg/L、0.5~50.0 μg/L或5.00~500 μg/L浓度范围内线性良好，相关系数为0.9921~0.9995，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。

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

Abstract:

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 tandem 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 T₃ column (100 mm×2.1 mm, 1.7 μm) utilizing a gradient elution program of methanol and water as the mobile phases at a flow rate of 0.2 mL/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 of 0.05-5.00 μg/L, 0.50-50.0 μg/L or 5.00-500 μg/L with correlation coefficients from 0.9921 to 0.9995. The limits of detection (LODs) for the nine perfluorinated compound precursors were in the ranges of 0.05-7.9 ng/L. The recoveries ranged from 76.0% to 106% with the relative standard deviations between 0.72% and 13.7%. 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.

Key words: atmospheric precipitation, perfluorinated compound precursors, solid phase extraction (SPE), ultra performance liquid chromatography-electrospray ionization-tandem mass spectrometry (UPLC-ESI MS/MS)

中图分类号:

O658

张明, 唐访良, 徐建芬, 余波, 张伟, 姚建良, 胡敏华. 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[J]. 色谱, 2017, 35(10): 1073-1079.

ZHANG Ming, TANG Fangliang, XU Jianfen, YU Bo, ZHANG Wei, YAO Jianliang, HU Minhua. Simultaneous determination of nine perfluorinated compound precursors in atmospheric precipitation by solid phase extraction and ultra performance liquid chromatography with tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2017, 35(10): 1073-1079.

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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

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