快速溶剂萃取-固相萃取-液相色谱-串联质谱法同时检测小型家用电器中溴代阻燃剂

卢晓宇; 张敬轩; 李挥; 张岩

doi:10.7538/zpxb.2013.34.02.0103

快速溶剂萃取-固相萃取-液相色谱-串联质谱法同时检测小型家用电器中溴代阻燃剂

Determination of Brominated Flame Retardants in the Household Appliances by ASE-SPE-RRLC-MS/MS

摘要

摘要: 建立了快速溶剂萃取-固相萃取-超快速液相色谱-串联质谱(ASE-SPE-RRLC-MS/MS)测定小型家用电器中溴代阻燃剂残留(六溴环十二烷(HBCDs)、四溴双酚A(TBBP-A))的方法。试样经冷冻粉碎后，以V（丙酮）∶V（正己烷）=1∶1的溶液为萃取液，采用快速溶剂萃取法,萃取液经C₁₈固相萃取柱富集净化，以水甲醇为流动相，经C₁₈柱分离后,以快速液相色谱串联质谱法多反应监测扫描模式进行定性和定量分析。方法的线性相关系数r大于0.998，检出限为0.05～0.2 mg/kg，在0.05～800 mg/kg等浓度添加水平下，平均回收率为87.72%～95.71%；相对标准偏差（RSD）为4.42%～8.38%。该方法灵敏度高、重现性好、定性定量准确，适用小型家用电器的复杂基质样品检测，可为相关国家标准制定提供参考依据。

Abstract: A accelerated solvent extraction-solid phase extraction rapid resolution liquid chromatography-tandem mass spectrometry (ASE-SPE-RRLC-MS/MS) method for the determination of brominated flame retardants （HBCDs，TBBP-A）in the household appliance was developed. V（acetone）∶V（hexane）= 1∶1 as an extraction solvent and accelerated solvent extraction method were been adopted. The brominated flame retardants in sample solution were separated and enriched by solid phase extraction (SPE) on C₁₈ column. The brominated flame retardants residue was separated by HPLC using methanol-water as the mobile phase，and was detective using electrospray ionization (ESI) on a tandem mass spectrometer in multiple reactions monitoring mode. The detection limits are 0.05—0.2 mg/kg, and the correlation coefficient is larger than 0.998. At the spiked level of 0.05—800 μg/kg, the recoveries are 87.72%—95.71%, and the relative standard deviations are in the range of 4.42% and 8.38%（n=10）. This method is sensitive, recurrent and accurate. It can be used for the determination of brominated flame retardants in the household appliances，and can provide reference for the relevant national standards setting.

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