Semiautomated high-throughput extraction and cleanup method for the measurement of polybrominated diphenyl ethers and polybrominated and polychlorinated biphenyls in breast milk
Semiautomated high-throughput extraction and cleanup method for the measurement of polybrominated diphenyl ethers and polybrominated and polychlorinated biphenyls in breast milk
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DOI：
10.1021/ac0495384
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发表时间：
2004-08-01
影响因子：
7.4
通讯作者：
Patterson, DG
中科院分区：
文献类型：
--
作者：
Sjodin, A;McGahee, EE;Patterson, DG
建立了测定8种多溴联苯醚(PBDEs)、2，2‘，4，4’，5，5‘-六溴联苯(BB-153)和2，2’，4，4‘，5，5’-六氯联苯(CB-153)的半自动萃取净化方法。该方法采用固相萃取柱中硅藻土上的固相分散，然后自动添加内标(C-13标记)。然后使用自动化的模块化固相萃取系统进行萃取。提取过程包括在硅藻土上加压氮气干燥样品，并用二氯甲烷洗脱目标分析物和脂类。脂肪含量是用重量法测定的。使用该方法进行的脂类测定与其他标准方法和标准物质进行了比较。对某母乳质控样品进行130次测定，相对标准偏差为7.9%。采用气相色谱-同位素稀释高分辨质谱法进行目标分析物的最终分析测定。对于浓度高于1 ng/g脂的分析物，对于具有标记内标的目标分析物的测量的相对标准偏差低于10%。对于8种多溴二苯醚同系物，13C标记内标的平均回收率在60%到89%之间；BB-153和CB-153的平均回收率分别为74%和113%。
A semiautomated extraction and cleanup method has been developed to measure eight polybrominated diphenyl ethers (PBDEs), 2,2',4,4',5,5'-hexabromobiphenyl (BB-153), and 2,2',4,4',5,5'-hexachlorobiphenyl (CB-153). The method employs solid-phase dispersion on diatomaceous earth in a solid-phase extraction cartridge followed by automated addition of internal standards (C-13-labeled). Extraction is then performed using an automated modular solid-phase extraction system. The extraction procedure includes drying the sample on diatomaceous earth by pressurized nitrogen and eluting target analytes and lipids with dichloromethane. Lipid content is determined gravimetrically. Lipid determinations performed using this method are compared with other standard methods and with a certified reference material. A relative standard deviation of 7.9% was obtained for 130 determinations of the lipid content in a breast milk quality control sample. Final analytical determination of target analytes was performed by gas chromatography-isotope dilution high-resolution mass spectrometry. Relative standard deviations for the measurements of target analytes for which a labeled internal standard was available were below 10% for analytes at concentrations above 1 ng/g of lipid. Mean recoveries of the 13C-labeled internal standards ranged from 60 to 89% for the eight PBDE congeners; 74 and 113% were recovered for BB-153 and CB-153, respectively.