Optimization of the determination of polybrominated diphenyl ethers in human serum using solid-phase extraction and gas chromatography-electron capture negative ionization mass spectrometry
Optimization of the determination of polybrominated diphenyl ethers in human serum using solid-phase extraction and gas chromatography-electron capture negative ionization mass spectrometry
复制标题
DOI：
10.1016/j.jchromb.2005.09.020
复制
发表时间：
2005-12-05
影响因子：
3
通讯作者：
Voorspoels, S
中科院分区：
文献类型：
--
作者：
Covaci, A;Voorspoels, S
建立了一种简单、快速、灵敏、重现性好的固相萃取-酸化硅胶净化法测定人血清中12种多溴联苯醚（PBDEs），包括BDE 209和2，2 '，4，4，5，5'-六溴代二苯（BB 153）。测试了几种固相吸附剂（EmporeTM C-18、IsolutePheny、IsoluteENV+和OASISTM HLB），发现OASISTM HLB（500 mg）的绝对回收率最高（在64%和95%之间，R.S.D.）。<17%，n = 3）。使用含有（从下到上）硫酸浸渍的二氧化硅、活化二氧化硅和无水硫酸钠的6 ml一次性柱进行共提取生物源材料的去除。使用气相色谱仪和质谱仪（MS）以电子捕获负电离模式对多溴二苯醚和BB 153进行定量。方法定量限（LOQ）范围为0.2至25 pg/ml血清（0. 1和4纳克/克脂重）。LOQ取决于程序空白中的分析物水平，这导致在空白中发现的浓度较高的多溴二苯醚同系物（例如BDE 47、99和209）的LOQ最高。使用OASIS（TM）HLB固相萃取柱可实现良好的方法重复性（除BDE 209 <17%外，所有同系物的日内和日间精确度< 12%，n = 3）。该方法应用于来自比利时随机人群的血清样本。所获得的结果在欧洲其他未接触多溴二苯醚人群的多溴二苯醚水平范围内。(c)2005 Elsevier B. V.保留所有权利。
A simple, rapid, sensitive and reproducible method based on solid-phase extraction (SPE) and acidified silica clean-up was developed for the measurement of 12 polybrominated diphenyl ethers (PBDEs), including BDE 209, and 2,2',4,4,5,5'-hexabromobiphenyl (BB 153) in human serum. Several solid-phase sorbents (Empore (TM) C-18, Isolute Pheny], Isolute ENV+ and OASIS (TM) HLB) were tested and it was found that OASIS (TM) HLB (500 mg) gives the highest absolute recoveries (between 64% and 95%, R.S.D. < 17%, n = 3) for all tested analytes and internal standards. Removal of co-extracted biogenic materials was performed using a 6 ml disposable cartridge containing (from bottom to top) silica impregnated with sulphuric acid, activated silica and anhydrous sodium sulphate. PBDEs and BB 153 were quantified using a gas chromatograph coupled with a mass spectrometer (MS) operated in electron-capture negative ionization mode. The method limits of quantification (LOQ) ranged between 0.2 and 25 pg/ml serum (0. 1 and 4 ng/g lipid weight). LOQs were dependent on the analyte levels in procedural blanks which resulted in the highest LOQs for PBDE congeners found in higher concentrations in blanks (e.g. BDE 47, 99 and 209). The use of OASIS (TM) HLB SPE cartridge allowed a good method repeatability (within- and between-day precision < 12% for all congeners, except for BDE 209 < 17%, n = 3). The method was applied to serum samples from a random Belgian population. The obtained results were within the range of PBDE levels in other non-exposed population from Europe. (c) 2005 Elsevier B.V. All rights reserved.