建立了固相萃取-超高效液相色谱-电喷雾串联三重四极杆质谱联用技术分析水中16种全氟有机化合物的高通量检测方法。样品经 WAX 固相萃取柱富集和净化后，采用 Waters ACQUITY UPLCTM BEH C18色谱柱，含2 mmol/L乙酸铵的甲醇和含2 mmol/L乙酸铵的水作为流动相进行梯度洗脱，质谱采用电喷雾负离子电离，多反应监测模式检测。16种全氟有机化合物在0.5~100μg/L或1.0~100μg/L 浓度范围内线性关系良好，相关系数为0.9987~0.9999，方法的检出限为0.06~0.46 ng/L；高、中、低3个添加水平的回收率为67.6％~103％，相对标准偏差为2.94％~12.0％。结果表明，该方法灵敏、准确且检测范围广，分析速度快，是一种适于实际水样中全氟有机化合物检测分析的方法。
A high-throughput detection method has been developed for the determination of six-teen perfluorinated organic compounds( PFCs)in surface water by solid phase extraction-ultra performance liquid chromatography coupled with electrospray ionization tandem mass spec-trometry( SPE-UPLC-ESI-MS/MS). The water samples were concentrated and purified through WAX solid phase extraction cartridges. The UPLC separation was performed on an ACQUITY UPLCTM BEH C18 column utilizing a gradient elution program of methanol(containing 2 mmol/L ammonium acetate)and water( containing 2 mmol/L ammonium acetate)as the mobile phases at a flow rate of 0. 4 mL/min. The MS/MS detection was performed under negative electrospray ionization( ESI-)in multiple reaction monitoring( MRM)mode. Good linearities were observed in the range of 0. 5-100 μg/L or 1. 0-100 μg/L with correlation coefficients from 0. 998 7 to 0. 999 9. The limits of detection( LODs)for the sixteen perfluorinated organic compounds were in the range of 0. 06-0. 46 ng/L. The recoveries ranged from 67. 6% to 103% with the relative standard deviations between 2. 94% and 12. 0%. This method was characterized by high sensitiv-ity and precision,extensive range and high speed,and can be applied for the analysis of PFC contaminants in surface water.
参考文献
| [1] | Paul A G;Jones K C;Sweetman A J.[J].Environmental Science and Technology,200943(02):386. |
| [2] | Ahrens L;Shoeib M;Harner T.[J].Environmental Science and Technology,201145(19):8098. |
| [3] | Prevedouros K;Cousins I;Buck R.[J].Environ Sci Tech-nol,200640(01):32. |
| [4] | Rayne S;Forest K.[J].J Environ Sci Health Part A,200944:1145. |
| [5] | Ahrens L.[J].Journal of Environmental Monitoring,201113(01):20. |
| [6] | Lau C;Anitole K;Hodes C.[J].Toxicological Sciences,200799:366. |
| [7] | Giesy J P;Naile J E;Khim J S.[J].Reviews of Environmental Contamination and Toxicology,2010202:1. |
| [8] | Eschauzier C;Beerendonk E;Scholte-Veenendaal P.[J].Environmental Science and Technology,201246(03):1708. |
| [9] | 彭思远;严丽娟;张洁.[J].色谱,201230(02):123. |
| [10] | United Nations Environment Programme(UNEP).UNEP-POPS-COP.4-SC-4-17.Listing of Perfluorooctane Sulfonic Acid,Its Salts and Perfluorooctane Sulfonyl Fluoride[A].Geneva,2009-05-09 |
| [11] | 陈春丽;王铁宇;吕永龙.[J].环境科学,201132(04):1073. |
| [12] | 陈静;王琳玲;朱湖地.[J].环境科学,201233(08):2586. |
| [13] | Zhang W;Zhang Y T;Taniyasu S.[J].Environmental Pollution,2013176:10. |
| [14] | 彭蓉;程小艳;张克荣.[J].四川环境,200827(03):97. |
| [15] | 王利兵;吕刚;刘绍从.[J].分析试验室,200726(02):94. |
| [16] | 赵晓峰;李云;张海军.[J].色谱,201028(05):435. |
| [17] | 张明;唐访良;陈峰.[J].色谱,201230(01):51. |
| [18] | 郑海;胡国成;许振成.[J].农业环境科学学报,201332(04):778. |
| [19] | 章涛;孙红文;Alder Alfredo C.[J].色谱,201028(05):498. |
| [20] | 张萍;史亚利;蔡亚岐.[J].分析化学,200735(07):969. |
| [21] | 王传现;郭德华;李波.[J].卫生研究,200736(06):727. |
| [22] | 李鑫;陈军辉;程红艳.[J].环境化学,201231(06):896. |
| [23] | US EPA .Title 40:Part 136,Appendix B to Part 136[OL].http://www.gpo.gov/fdsys/pkg/CFR-2011-title40-vol23/pdf/CFR-2011-title40-vol23-part136-appB.pdf,1986-06-30. |
| [24] | US EPA .Provisional Health Advisories for Perfluorooctanoic Acid (PFOA) and Perfluorooctane Sulfonate (PFOS)[OL].http://water.epa.gov/action/advisories/drinking/upload/2009 01 15 criteria drinking pha-PFOA PFOS.pdf,2009-01-15. |
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