| 尿液中12种全氟化合物的固相萃取-超高效液相色谱串联四极杆线性离子阱质谱分析方法研究 |
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| 引用本文： | 罗新月,赵璇,任琳,王文佳,雍莉,袁悦,曾红燕,邹晓莉. 尿液中12种全氟化合物的固相萃取-超高效液相色谱串联四极杆线性离子阱质谱分析方法研究[J]. 四川大学学报(医学版), 2021, 52(4): 679-685. DOI: 10.12182/20210760504 |
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| 作者姓名： | 罗新月 赵璇 任琳 王文佳 雍莉 袁悦 曾红燕 邹晓莉 |
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| 作者单位： | 四川大学华西公共卫生学院/四川大学华西第四医院 卫生检验与检疫系 成都 610041;四川省疾病预防控制中心 成都 610041 |
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| 基金项目： | 国家重点研发计划项目（No. 2017YFC1600200）和四川省科技厅重点研发项目（No. 2020YFS0056）资助 |
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| 摘 要： | 目的 建立超高效液相色谱串联四极杆线性离子阱质谱同时测定尿液中12种全氟化合物(PFCs)的方法.方法 尿样经2％甲酸调节pH后,用WAX柱萃取净化浓缩,收集洗脱液氮吹,10 mmol/L乙酸铵-甲醇(V水:V甲=70:30)复溶,离心取上清液进样分析.超高效液相色谱采用甲醇和10 mmol/L乙酸铵水溶液在C18柱上...
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| 关 键 词： | 全氟化合物 尿液 固相萃取法 超高效液相色谱串联四极杆线性离子阱质谱法 |
| 收稿时间： | 2020-08-07 |
Study on the Analytical Method of Solid Phase Extraction-Ultra Performance Liquid Chromatography Tandem Quadrupole Linear Ion Trap Mass Spectrometry for 12 Perfluorinated Compounds in Human Urine |
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| LUO Xin-yue,ZHAO Xuan,REN Lin,WANG Wen-jia,YONG Li,YUAN Yue,ZENG Hong-yan,ZOU Xiao-li. Study on the Analytical Method of Solid Phase Extraction-Ultra Performance Liquid Chromatography Tandem Quadrupole Linear Ion Trap Mass Spectrometry for 12 Perfluorinated Compounds in Human Urine[J]. Journal of Sichuan University. Medical science edition, 2021, 52(4): 679-685. DOI: 10.12182/20210760504 |
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| Authors: | LUO Xin-yue ZHAO Xuan REN Lin WANG Wen-jia YONG Li YUAN Yue ZENG Hong-yan ZOU Xiao-li |
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| Affiliation: | 1.Department of Laboratory Technology and Science of Public Health, West China School of Public Health and West China Fourth Hospital, Sichuan University, Chengdu 610041, China |
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| Abstract: | Objective To establish a method for simultaneous determination of 12 kinds of perfluorinated compounds (PFCs) in human urine based on ultra performance liquid chromatography tandem quadrupole linear ion trap mass spectrometry (UPLC-QTtrap-MS). Methods After pH adjustment with 2% formic acid, the urine samples were loaded on a WAX solid phase extraction (SPE) cartridge for extraction, purification and concentration. The eluates were collected, concentrated to dryness under nitrogen, and reconstituted with 10 mmol/L ammonium acetate aqueous solution-methanol (Vwater∶Vmethanol = 70∶30) before injection. UPLC was performed on a C18 cartridge, and methanol and 10 mmol/L ammonium acetate aqueous solution was used as mobile phases with gradient elution. QTtrap-MS was operated in multiple reaction monitoring (MRM) mode, and the internal standard calibration curves were applied for quantitative analysis. Results Good linearity was obtained in the linear range, with the method detection limits and method quantification limits being 0.032 ng/L-6.5 ng/L and 0.10 ng/L-21 ng/L, respectively, for the 12 kinds of PFCs. The spiked recoveries of the 12 kinds of PFCs were 91.5%-114%, with the intra-day precision and the inter-day precision being 0.57%-16.0% and 1.88%-20.1%, respectively. The established method was applied to the determination of 12 kinds of PFCs in the urine samples of primary school students collected in one area. Nine kinds of PFCs were detected in the urine samples in this area. Among the PFCs detected, perfluorobutanesulfonic acid (PFBS) and perfluorooctanoic acid (PFOA) were the main PFCs found in the student urine samples. Conclusion The method established in this study could be used to simultaneously examine 12 kinds of PFCs in urine. The method combined SPE with isotope internal standard correction and achieved good sensitivity and accuracy. |
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