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《化学分析计量》 2020年第01期
DOI:10.3969/j.issn.1008-6145.2020.01.015
高效液相色谱-串联质谱法检测环境水体中18 种全氟化合物
杨文宇1,赵慧2,钟琳1,李支薇1
(1. 广州广电计量检测股份有限公司,广州 510656; 2.中车长春轨道客车股份有限公司,长春 130062) 
Determination of 18 perfluorinated alkyl substances in environmental water by high performance liquid chromatography-tandem mass spectrometry
杨文宇1,赵慧2,钟琳1,李支薇1
(1. Guangzhou GRG Metrology & Test Co., Ltd., Guangzhou 510656, China;
2. CRRC Changchun Railway Vehicles Co., Ltd., Changchun 130062, China) 
摘要:建立了快速检测环境水体中18 种全氟化合物的高效液相-串联质谱方法。环境水样经大体积PEP 固相 萃取柱快速提取、富集和净化后,过0.22 μm 微孔滤膜,再利用Agilent Zorbax Eclipse XDB-C18反相色谱柱分离,以5 mmol/L 乙酸铵溶液和甲醇为流动相梯度洗脱,最终进入电喷雾离子源负离子扫描,在多反应监测模式下定性及定 量分析。所有目标化合物的质量浓度在1~20 μg/L 范围内与色谱峰面积线性良好,相关系数(r2) 大于0.999,方法 检出限为0.18~0.48 ng/L。18 种全氟化合物的加标回收率为90.1%~107.3%,相对标准偏差为0.3%~8.2% (n=6)。 该方法操作简单、快速,灵敏度高,可满足环境水体中全氟化合物的检测。 
Abstract:A method was established for the determination of 18 perfluorinated alkyl substances (PFASs) in environmental water by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The environmental water sample was quickly extracted, enriched and cleaned-up by PEP solid phase extraction, then filtered through 0.22 μm microporous membrane; the separation of 18 PFASs was performed on an Agilent Zorbax Eclipse XDB- C18 column using gradient elution of 5 mmol/L ammonium acetate and methanol as mobile phase. PFASs were analyzed under the multiple reaction monitoring (MRM) mode with negative electrospay ionization. The calibration curves of all PFASs had a good linear relationship with the chromatographic peak area in the range of 1-20 μg/L with the correlation coefficients (r2) more than 0.999. The detection limits ranged from 0.18 ng/L to 0.48 ng/L. The spiked recoveries for 18 PFASs were between 90.1% and 107.3% with the relative standard derivations from 0.3% to 8.2% (n=6). The developed method is simple, rapid and sensitive, and it is suitable for rapid analysis of PFASs in environmental water. 
关键词:全氟化合物;高效液相-串联质谱法;大体积固相萃取;环境水体 
Keywords:perfluorinated alkyl substances; high performance liquid chromatography-tandem mass spectrometry; large volume solid phase extraction; environmental water 
本文引用格式:
杨文宇,赵慧,钟琳,等. 高效液相色谱- 串联质谱法检测环境水体中18 种全氟化合物[J]. 化学分析计量,2020,29(1):61-66.
YANG W Y,ZHAO H,ZHONG L,et al. Determination of 18 perfluorinated alkyl substances in environmental water by high performance liquid chromatography-tandem mass spectrometry[J]. Chemical analysis and meterage,2020,29(1):61-66. 

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