摘要
目的建立了固相萃取(SPE)柱萃取和净化、超高效液相色谱-电喷雾离子源-串联质谱(UPLC-ESI--MS/MS)检测血液中11种羟基多溴联苯醚(OH-PBDEs)的方法。方法对流动相和SPE萃取条件进行了优化。结果人血液加标回收率53.2%～117.9%,相对标准偏差4.71%～18.85%,检出限0.008 86～0.058 9 ng/ml。结论本方法不需要衍生化,灵敏度高、准确度和精密度好,简便快速,溶剂消耗量少,适用于人血样品中羟基多溴联苯醚的测定。
Objective A simplified analytical method comprised of solid-phase extraction （SPE） and ultra performance liquid chromatography coupled with negative electrospray ion source tandem mass spectrometry （UPLC-ESI-MS/MS） has been developed for the determination of eleven hydroxylated polybrominated diphenyl ethers （OH-PBDEs） in human blood. Methods The solvent for the mobile phase and the SPE conditions were optimized. Results The recoveries of the OH- PBDEs spiked in human blood relative to internal standards were in the range of 53.2%-117.9% at three spiked levels. The relative standard deviations （RSD） were 4. 71%-18.85%. The limits of detection （LOD, S/N=3） was in the range of 0.00886-0.058 9 ng/ml. Conclusion The proposed method is sensitive, accurate, fast, simple, low solvent consumption and suitable for the determination of OH-PBDEs in human serum without derivatization.
出处
《中国食品卫生杂志》
北大核心
2012年第4期317-321,共5页
Chinese Journal of Food Hygiene
基金
国家自然科学基金(20907048)
卫生公益性科研专项(200902009)
湖北省卫生厅青年人才(QJX-2010-33)
