加速溶剂同时萃取和净化-气相色谱-三重四极杆串联质谱测定土壤和沉积物中8种多溴联苯醚

建立了土壤和沉积物中8种多溴联苯醚(PBDEs,BDE-28、BDE-47、BDE-99、BDE-100、BDE-153、BDE-154、BDE-183和BDE-209)加速溶剂同时萃取和净化-气相色谱-三重四极杆串联质谱(ASE-GC-MS-MS)的分析方法。通过优化加速溶剂萃取与弗罗里硅土在线净化和串联质谱多反应监测模式的条件,较好地去除基质干扰,并提高了三重四极杆串联质谱定性的准确性及定量的灵敏性。该方法采用改进的色谱柱能同时分析包括高溴代联苯醚BDE-209在内的8种PBDEs,其浓度范围为1～100 ng/mL(BDE-209为10～1 000 ng/mL),线性良好,线性回归系数均大于0.997。方法检出限为0.004～0.1 ng/g,方法回收率为75%～110%,方法精密度为2.4%～15.6%。适于批量处理土壤和沉积物中含有多组分痕量PBDEs的样品。

Determination of 8 PBDEs in Soil and Sediment by Accelerated Solvent Simultaneous Extraction and Clean-Up with Gas Chromatography-Triple Quadrupole Mass Spectrometry

A synchronous extraction and purification method using accelerated solvent extraction gas chromatography-triple quadrupole mass spectrometry was developed for the determination of eight polybrominated diphenyl ethers (PBDEs) in soil and sediment, including BDE-28, BDE-47, BDE-99, BDE-100, BDE-153, BDE-154, BDE-183 and BDE-209. The samples from optimization for accelerated solvent extraction were purified by on-line clean-up of activated Florisil during PBDE extraction, combined with the multiple-reaction monitor modes of tandem mass spectrometry, so the background disturbing noise was reduced a lot and the qualitative and quantitative accuracy was improved. Eight PBDEs including high brominated diphenyl ethers (BDE-209) were analyzed synchronously by using improved chromatographic column, The good linear relationships were obtained with coefficient more than 0.997 in the range of 1 ng/mL to 100 ng/mL (10-1000 ng/mL for BDE-209)for eight PBDEs. The method detection limit, recoveries and relative standard deviation ranged from 0.004-0.1 ng/g, 75% to 110% and 2.4% to 15.6%, respectively. This method was suitable for processing a large batch of samples of trace PBDEs in soil and sediment.