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预防医学  2020, Vol. 32 Issue (12): 1204-1207    DOI: 10.19485/j.cnki.issn2096-5087.2020.12.004
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超高效液相色谱-串联质谱法测定鱼肉全氟羧酸化合物
刘少颖, 金铨, 任韧, 黄希汇
杭州市疾病预防控制中心,浙江 杭州 310021
Determination of perfluorocarboxylic acids in fish by ultra performance liquid chromatography tandem mass spectrometry
LIU Shaoying, JIN Quan, REN Ren, HUANG Xihui
Hangzhou Center for Disease Control and Prevention, Hangzhou, Zhejiang 310021, China
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摘要 目的 建立超高效液相色谱-串联质谱法测定鱼肉中9种全氟羧酸化合物(PFCAs)。方法 鱼肉样品经甲基叔丁基醚萃取,WAX固相萃取柱净化,使用甲醇和25 mmol/L乙酸铵溶液依次淋洗,0.5%氨水甲醇洗脱,氮吹至近干后,50%甲醇水溶液复溶,选择1 mmol/L乙酸铵水溶液-甲醇作为流动相,采用超高效液相色谱-串联质谱法检测分析。结果 9种PFCAs在UPLC BEH-C18色谱柱上能较好分离,在1.0~200.0 ng/mL范围线性关系良好,相关系数>0.99,检出限为0.06~0.19 µg/kg,定量限为0.19~0.62 µg/kg。在5.0、25.0、50.0 μg/kg水平的回收率为70.08%~117.24%,相对标准偏差为2.31%~19.68%。结论 通过优化预处理条件,液相色谱流动相和质谱检测条件建立的超高效液相色谱-串联质谱法适用于鱼肉中全氟羧酸化合物测定。
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刘少颖
金铨
任韧
黄希汇
关键词 超高效液相色谱-串联质谱鱼肉全氟羧酸化合物    
AbstractObjective To develop the ultra performance liquid chromatography tandem mass spectrometry ( UPLC-MS/MS ) for the determination of perfluorocarboxylic acids ( PFCAs ) in fish. Methods The fish samples were extracted with tert-butyl methyl ether and purified by WAX columns. The WAX cartridges were rinsed with methanol and 25 mmol/L ammonium acetate, and the target compound residues were eluted with 0.5% ammonia methanol and then redissolved with 50% methanol aqueous solution after nitrogen blowing to nearly dry. Nine kinds of PFCAs were simultaneously quantified by UPLC-MS/MS with 1 mmol/L ammonium acetate-methanol solution as the mobile phase. Results The extraction was separated well in UPLC BEH C18 column. There were good linear correlations of nine kinds of PFCAs in the range of 1.0-200.0 ng/mL, with the coefficients all more than 0.99. The limits of detection and quantification were 0.06-0.19 μg/kg and 0.19-0.62 μg/kg, respectively. The recovery rates were 70.08%-117.24% at different spiked levels ( 5.0, 25.0, 50.0 μg/kg ), and the relative standard deviations were 2.31%-19.68%. Conclusion Through optimizing the pretreatment conditions, the mobile phase of liquid chromatography and the detection conditions of mass spectrometry, the UPLC-MS/MS could meet the monitoring requirements of PFCAs in fish.
Key wordsultra performance liquid chromatography tandem mass spectrometry    fish    perfluorocarboxylic acids
收稿日期: 2020-09-01      修回日期: 2020-10-21     
中图分类号:  R123.1  
基金资助:浙江省分析测试科技计划项目(2018C37031)
通信作者: 金铨,E-mail:jinquanjinquan@163.com   
作者简介: 刘少颖,博士,副主任技师,主要从事理化分析工作
引用本文:   
刘少颖, 金铨, 任韧, 黄希汇. 超高效液相色谱-串联质谱法测定鱼肉全氟羧酸化合物[J]. 预防医学, 2020, 32(12): 1204-1207.
LIU Shaoying, JIN Quan, REN Ren, HUANG Xihui. Determination of perfluorocarboxylic acids in fish by ultra performance liquid chromatography tandem mass spectrometry. Preventive Medicine, 2020, 32(12): 1204-1207.
链接本文:  
http://www.zjyfyxzz.com/CN/10.19485/j.cnki.issn2096-5087.2020.12.004      或      http://www.zjyfyxzz.com/CN/Y2020/V32/I12/1204
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