Online solid phase extraction-high performance liquid chromatography-inductively coupled plasma mass spectrometry (Online SPE-HPLC-ICP-MS) technique was developed for simultaneous determination of 6 kinds of polybrominated diphenyl ethers and 5 kinds of hydroxyl metabolites in serum. A serum sample (200 μL) was directly analyzed after protein precipitation and dilution. The target analytes were automatically enriched on a solid phase extraction column, and then separated and analyzed by liquid chromatography-inductively coupled plasma mass spectrometry with methanol/acetonitrile/water as mobile phase. The main parameters such as loading rate, elution time and elution solvent were optimized. As a result, Oasis HLB was selected as the SPE column, the loading solvent was pure water at a rate of 3.0 mL/min, the elution solvent was methanol-acetonitrile-water (54:26:20, V/V), the elution flow rate was 1.0 mL/min, and the liquid chromatography column was ZORBAX Eclipse Plus C₁₈. The limits of quantification (LOQ) of the method were 0.14–0.74 ng/L, the recoveries were 61.8%–77.7%, and the relative standard deviations (RSDs) of the results were 3.7%–10.1% (n = 3). The established method was successfully applied to the analysis of 30 serum samples. A total of 4 kinds of polybrominated diphenyl ethers and 2 kinds of hydroxy polybrominated diphenyl ethers were detected, and their occurrence characteristics were consistent with previous reports. The results showed that this method could be applied to analyze actual samples in large quantities, which was of great practical value.

建立了在线固相萃取-高效液相色谱-电感耦合等离子体质谱（在线SPE-HPLC-ICP-MS）技术，用于同时测定血清中6种多溴联苯醚和5种羟基代谢物的方法。蛋白质沉淀和稀释后，直接分析血清样品（200μL）。在固相萃取柱上自动富集目标分析物，然后通过液相色谱-电感耦合等离子体质谱法（以甲醇/乙腈/水为流动相）进行分离和分析。优化了负载率，洗脱时间和洗脱溶剂等主要参数。结果，选择了Oasis HLB作为SPE色谱柱，上样溶剂为纯水，流速为3.0 mL / min，V / V），洗脱流速为1.0 mL / min，液相色谱柱为ZORBAX Eclipse Plus C ₁₈。该方法的定量限（LOQ）为0.14-0.74 ng / L，回收率为61.8％-77.7％，结果的相对标准偏差（RSD）为3.7％-10.1％（n = 3）。所建立的方法已成功地用于30个血清样品的分析。共检测出4种多溴联苯醚和2种羟基多溴联苯醚，其发生特征与以前的报道相符。结果表明，该方法可用于大量实际样品的分析，具有很大的实用价值。