| 水中全氟烷基醚类羧酸的超高效液相色谱－串联质谱检测方法研究 |
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| 基金项目:国家自然科学基金项目（31972145）；齐鲁工业大学（山东省科学院）青年博士合作基金项目（2019BSHZ0029）；山东省重点研发计划（重大科技创新工程）（2021CXGC010508） |
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| 中文摘要:电喷雾离子源条件下全氟烷基醚类羧酸（PFECA）发生源内裂解和CO2中性丢失，导致其准分子离子峰的丰度降低，影响该类化合物的检测灵敏度。该文选择［CF3（CF2）nO］或［M－H－CO2］作为母离子，其他次级氟化烷氧基和烷基片段作为子离子，可将全氟烷基醚类羧酸的质谱响应最大提高4个数量级。结合液液萃取，对水样中4种全氟烷基醚类羧酸进行超高效液相色谱－串联质谱检测。4种PFECA均具有良好的线性关系，相关系数（r2）均大于0.99，检出限和定量下限分别为0.001～0.005 ng/mL和0.003～0.01 ng/mL，加标回收率为90.2%～108%，相对标准偏差（RSD）不大于7.9%。该方法为PFECA的准确定量、高灵敏检测提供了依据。 |
| 中文关键词:全氟烷基醚类羧酸（PFECA） 超高效液相色谱 质谱 源内裂解 CO2中性丢失 |
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| Analysis of Perfluoroalkyl Ether Carboxylic Acid in Water by Ultra- performance Liquid Chromatography－Tandem Mass Spectrometry |
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| Abstract:The abundance of excimer ion peaks could be decreased by the in?source fragmentation and neutral loss of molecule CO2 occurred within perfluoroalkyl ether carboxylic acids（PFECAs） under ESI source，which affects the detection sensitivity for PFECA. In this paper，［CF3（CF2）nO］ or ［M－H－CO2］ was selected as the parent ion，and fluorinated alkoxy and alkyl groups were selected as the daughter ions，which could increase the response of PFECAs by 4 orders of magnitude at most. Four PFECAs in water samples were detected by ultra?performance liquid chromatography－tandem mass spectrometry combined with liquid－liquid extraction. There were good linear relationships for the four analytes with their correlation coefficients（r2） larger than 0.99. The limits of detection and limits of quantitation were in the range of 0.001－0.005 ng/mL and 0.003－0.01 ng/mL，respectively. The spiked recoveries ranged from 90.2% to 108%，with relative standard deviations（RSD） not more than 7.9%. The method provides a platform for the accurate quantification and high sensitive detection of PFECAs. |
| Key Words:perfluoroalkyl ether carboxylic acid（PFECA） ultra?performance liquid chromatography mass spectrometry in?source fragmentation neutral loss of molecule CO2 |
| 引用本文：宋鑫,王荣雨,王晓,纪文华.水中全氟烷基醚类羧酸的超高效液相色谱－串联质谱检测方法研究[J].分析测试学报,2022,41(1):136-142. |
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