加速溶剂萃取-高效液相色谱法测定塑料制品中多溴二苯醚
HPLC Determination of Polybromodiphenyl Ether in Plastic Products with Accelerated Solvent Extraction of Sample
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摘要: 提出了塑料制品中多溴二苯醚的高效液相色谱法。样品经粉碎后用乙醇-丙酮(1+1)萃取溶剂经加速溶剂萃取仪在150 ℃静态萃取10 min,提取液旋转蒸发后用正己烷溶解过硅胶固相萃取柱净化,流出液蒸发至近干用异辛烷-甲苯(4+1)混合溶剂定容后,注入高效液相色谱仪分离测定。方法的检出限(3S/N)在0.1~0.2 mg·L-1之间,加标回收率在87%~104%之间。Abstract: Sample of plastic product was crushed and extracted with ethanol-acetone (1+1) solution under static condition at 150 ℃ for 10 min. The polybromodiphenyl ethers (PBDE) were dissolved in the organic phase and separated from the plastic matrix. The extract was evaporated to near dryness by rotary evaporator. The residue was dissolved with n-hexane and purified by silica gel solid-phase extraction. The eluate collected was evaporated to near dryness, and the residue was taken up with mixed solvent of isooctane and methylbenzene (4+1) and used for HPLC analysis. Values of detection limits (3S/N) of the method were found in the range of 0.1-0.2 mg·L-1 and values of recovery found by standard addition method were in the range of 87%-104%.