Abstract：Objective A high sensitivity method for determination of bisphenols in water by liquid chromatography-tandem mass spectrometry (LC-MS/MS) with solid phase extraction (SPE) was established. Methods The water samples were concentrated and purified by C18 cartridge directly, and then gradiently eluted with acetonitrile-water as the mobile phase for the baseline separation of the four compounds, bisphenol F (BPF), bisphenol A (BPA), tetrachlorobisphenol A (TCBPA ) and tetrabromobisphenol A (TBBPA), in thirteen minutes. BPA–d16 and TBBPA–d10 were used as internal standards and the analytes were identified by LC-MS/MS with the negative electrospray ionization under multiple reaction monitoring mode. Results The linear ranges of BPF, BPA, TCBPA and TBBPA in water all fell in 10ng/L-2,500ng/L. The linear correlation coefficients of their standard curves were 0.998, 0.998, 0.9998 and 0.9990 respectively, and the detection limits were 5ng/L, 2ng/L, 0.2ng/L and 2ng/L. The average recoveries for BPF, BPA, TCBPA and TBBPA at spiked concentration levels of 250 ng/L and 1000 ng/L were in the range of 65.3%~100.4%. Conclusions The LC-MS/MS coupled with SPE is simple, highly sensitive and selective. It provides an effective approch for the detection of bisphenols in water.
毛丽莎, 刘桂华, 姜杰, 刘红河, 康莉. 固相萃取-LC-MS/MS测定水中双酚A类物质[J]. 实用预防医学, 2016, 23(10): 1260-1263.
MAO Li-sha, LIU Gui-hua , JIANG Jie, LIU Hong-he, KANG Li. Determination of bisphenol A analogs in water sample by liquid chromatography-tandem mass spectrometry with solid phase extraction. , 2016, 23(10): 1260-1263.
[1] Pasquet C,Vulliet E. Utilisation of an enzyme-linked immunosorbent assay ( ELISA) for determination of alkylphenols in various environmental matrices. Comparison with LC-MS /MS method[J].Talanta,2011,(85):2492-2497. [2] 国先芬,王贻鑫,耿存珍,等.环境激素双酚A的毒理学研究进展[J].环境科学与技术,2013,36(2):86-92. [3] Kawaguchi M,Sakui N,Okanouchi N,et al. Stir bar sorptive extraction with in situ derivatization and thermal desorption-gas chromatography-mass spectrometry for measurement of phenolic xenoestrogens in human urine samples[J].J Chromatogr B Allalyt Technol Biomed Life Sci,2005,820(l):49-57. [4] 韩灏,邵兵,马亚鲁,等.高效液相色谱法测定饮料类食品中的类雌激素[J].色谱,2005, 23(2):176-179. [5] 范奇元,申立军,丁训诚,等.用子宫增重试验检测壬基酚的雌激素样作用[J].劳动医学,2000,17(4):196-197. [6] Khim Js,Lee KT,Kannan K,et al.Trace orgamic contaminants in sediment and water from Ulsan Bay and its vicinity,Korea[J].Arch Environ Contam Toxicol,2001,40: 141-150. [7] Heemken OP,Reincke H,Stachel B,et al.The occurrence of xenoestrogens in the Elbe river and the North Sea[J].Chermosphere,2001,45:245-259. [8] Inoue K, Kawaguchi M, Funakoshi Y, et al. Size-exclusion flow extraction ofbisphenol A in human urine for liquid chromatography-mass spectrometry[J]. J Chromatogr B Analyt Technol Biomed Life Sci,2003,798(l):17-23. [9] YE X, Kuklenyik Z,Needham LL,et al. Measuing environmental phenols and chlorinated organic chemicals in breast milk using automated on-line column-switching-high performance liquid chromatography-isotope dilution tandem masss spectrometry [J]. J Chromatogr B Analyt Technol Biomed Life Sci,2006,831(l-2):110-115. [10] 段醒妹,张晔.基质效应及其消除[J].赤峰学院学报(自然科学版),2000,2(1):17-18.
2016, Vol. 23 
