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.pdfVIP

PTCA (PART B: CHEM. ANAL.) 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 郑琳1 ，林力1 ，崔家玲1 ，王谦1 ，张海潮1 ，杨荣静2 ，韩旭l (1.宁波出入境检验检疫局，宁波 315012; 2. 上海出入境检验检疫局，上海 200135) 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 藻土混匀后采用丙嗣为溶剂，在 80 C , 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 经硅肢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 O. 005~60 mg. L -1 ，检出限(3SjN)在 O. 005~0. 03 mg • L -1 之间。方法用于聚丙烯、聚乙烯、丙烯睛-丁二烯-苯 乙烯塑料样品的分析，加标回收率在 83. 3% ~1l8% 之间，测定值的相对标准偏差Cn= 5) 在 3. 0%~9. 9%之间。 关键词:气相色谱-质谱法;加速溶剂革取;致敏芳香化合物;塑料 中固分类号: 0657.63 文献标志码:A 文章编号: 1001-4020(2015)02-0192-05 GC-MS Determination of 15 Fragrance Allergens in Plastics with Accelerated Solvent Extraction l l l l l ZHENG Linl , LIN Li , CUI Jia- Iing , WANG Qian , ZHANG Hai-chao , YANG Rong才ing2， HAN Xu (1. Ningbo Entr:yExit Insþection and Quarantine Bureau , Ningbo 315012 , China; 2. Shanghai Entr:yExit Insρection and Quarantine Bureau , Shanghai 200135 , China) Abstract: A method of GC-MS for the dete口nination 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 80C under pressure of 1 500 岛1Pa 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 colurnn before analysis. The analytes were quantified by internal standard method. Linearity ran