Xiao Qin, Hu Bin, Duan Jiankun, He Man, Zu Wanqing
Department of Chemistry, Wuhan University, Wuhan, China.
J Am Soc Mass Spectrom. 2007 Oct;18(10):1740-8. doi: 10.1016/j.jasms.2007.07.006. Epub 2007 Jul 17.
A novel method for the analysis of four polybrominated diphenyl ethers (PBDEs) in environmental and human serum samples based on hollow fiber-liquid phase microextraction (HF-LPME) followed by gas chromatography-inductively coupled plasma mass spectrometric (GC-ICP-MS) detection has been developed. The organic solvent in the porous hollow fiber was first dipped into the sample for extraction at a given time, and the retracted organic phase was introduced into the GC-ICP-MS for analysis. The addition of methanol has a strong effect on the HF-LPME extraction efficiency. Other significant parameters affecting the extraction efficiency of HF-LPME were also studied. HF-LPME was effective to isolate the analytes from the complex matrix. Under the optimized conditions, the detection limits of the proposed method varied from 15.2 to 40.5 ng/L. In general, the relative standard deviations (RSDs) were less than 10%. Good linearity was obtained with the correlation coefficients all better than 0.999. The proposed method is simple, quick, few microliters of organic solvent required, and is especially suitable for the analysis of the real sample with small amount available. The overall process of HF-LPME with GC-ICP-MS was applied successfully for the determination of polybrominated diphenyl ethers (PBDEs) in environmental and spiked human serum samples, and the results were satisfactory.
基于中空纤维液相微萃取(HF-LPME)结合气相色谱-电感耦合等离子体质谱(GC-ICP-MS)检测,开发了一种分析环境和人血清样品中四种多溴二苯醚(PBDEs)的新方法。首先将多孔中空纤维中的有机溶剂浸入样品中,在给定时间进行萃取,然后将缩回的有机相引入GC-ICP-MS进行分析。甲醇的添加对HF-LPME萃取效率有很大影响。还研究了其他影响HF-LPME萃取效率的重要参数。HF-LPME能有效地从复杂基质中分离出分析物。在优化条件下,该方法的检测限在15.2至40.5 ng/L之间。一般来说,相对标准偏差(RSDs)小于10%。获得了良好的线性关系,相关系数均优于0.999。该方法简单、快速,所需有机溶剂仅几微升,特别适用于分析少量实际样品。HF-LPME与GC-ICP-MS的整个过程成功应用于环境和加标人血清样品中多溴二苯醚(PBDEs)的测定,结果令人满意。