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    加速溶剂萃取-气相色谱-质谱法测定塑料中15种致敏芳香化合物

    GC-MS Determination of 15 Fragrance Allergens in Plastics with Accelerated Solvent Extraction

    • 摘要: 提出了加速溶剂萃取-气相色谱-质谱法测定塑料中15种致敏芳香化合物.样品与硅藻土混匀后采用丙酮为溶剂,在80 ℃,1 500 MPa压力条件下提取20 min,循环2次,萃取物浓缩定容后经DB-17石英毛细管色谱柱分离,在全扫描和选择离子监测模式下测定.颜色较深的样品经硅胶固相萃取小柱净化后测定,内标法定量.15种化合物的线性范围均为0.005~60 mg·L-1,检出限(3S/N)在0.005~0.03 mg·L-1之间.方法用于聚丙烯、聚乙烯、丙烯腈-丁二烯-苯乙烯塑料样品的分析,加标回收率在83.3%~118%之间,测定值的相对标准偏差(n=5)在3.0%~9.9%之间.

       

      Abstract: A method of GC-MS for the determination of 15 fragrance allergens in plastics with accelerated solvent extraction was proposed. The plastic sample was mixed with kieselguhr,then extracted for 20 min with acetone twice at 80℃ under pressure of 1 500 MPa. The extracts were separated on DB-17 quartz capillary chromatographic column,then determined under the full-scanning mode and the selected ion monitoring mode in MS. Deep color extract was cleaned up with a silica gel solid phase extraction column before analysis. The analytes were quantified by internal standard method. Linearity ranges of the 15 compounds were found between 0.005 mg·L-1 and 60 mg·L-1 with detection limit (3S/N) in the range of 0.005-0.03 mg·L-1. The proposed method was applied to the analysis of plastic samples of polypropylene,polyethylene and acrylonitrile butadiene styrene copolymers,giving values of recovery and RSD′s (n=5) in the ranges of 83.3%-118% and 3.0%-9.9%,respectively.

       

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