气质联用法测定纺织品中1-溴丙烷的含量
2015-05-25林宁婷连秋燕邱丽君杨瑜榕
林宁婷+连秋燕+邱丽君+杨瑜榕



摘要:本文建立了纺织品中1-溴丙烷的气相色谱-质谱(GC-MS)检测方法。本方法中样品经丙酮超声提取后,采用气相色谱-质谱联用全扫描和选择离子扫描方式对提取液进行定性定量分析,外标法定量。结果表明:在0.5 ~ 50.0 mg/L范围内,方法的线性关系良好,相关系数达0.999以上;方法检测低限为0.5 mg/kg,定量限为1.0 mg/kg;在1.0、2.0和10.0 mg/kg 3个加标水平下,回收率为82.0% ~ 95.0 %,相对标准偏差3.1% ~6.2%。
关键词:纺织品;1-溴丙烷;气相色谱-质谱联用法
中图分类号:TS107;O657.63 文献标志码:A
Determination of the Content of 1-Bromopropane in Textiles via Gas Chromatography-mass Spectrometric Method
Abstract: In this paper a gas chromatography-mass spectrometric (GC-MS) method was established for the determination of 1-Bromopropane (1-BP) in textiles. 1-Bp in textiles was extracted by ultrasound with Acetone, the ultimate solution was analyzed by GC-MS under full-scan and selected-ion monitoring mode and quantified by external standard method. The results showed that, in the range of 0.5 mg/L ~ 50.0 mg/L, the calibration curve was linear well with good correlation coefficients (R>0.999); the detection limit was 0.5 mg/kg and the limit of quantitation was 1.0mg/kg; the average recovery was 82.0% ~ 95.0%, and the relative standard deviations (RSD) were 3.1% ~ 6.2% at three spiked concentration levels of 1.0, 2.0, 10mg/kg.
Key words: textiles; 1-Bromopropane; gas chromatography-mass spectrometric method (GC-MS)
1-溴丙烷(1-Bromopropane,1-BP)又名溴代正丙烷,为无色液体,由溴化氢和丙醇经催化合成而得,主要用作溶剂,并且作为化工原料用于染料、阻燃剂、农药等的生产以及粘胶、涂料的配制,如王德虎等利用溴丙烷为起始原料合成一种易洗涤的活性染料。1-溴丙烷具有神经毒性和生殖毒性,欧盟化学品管理局于2012年12月19日正式将其列入高度关注的物质名单中。目前国内外对1-溴丙烷的检测主要集中在环境空气领域,已经报道的检测方法为气相色谱-氢火焰检测器法(FID)。至今为止,纺织品中1-溴丙烷的检测方法仍未见报道,也未见采用气质联用法测定1-溴丙烷的检验方法,亦未制订相应的国家纺织标准。本文采用气相色谱-质谱联用法,探索建立了一种纺织品中1-溴丙烷的检测方法,该方法具有前处理简单,定性定量准确,灵敏度高,稳定性好等特点,适用于纺织品中1-溴丙烷的分析测定,拓展了纺织品生态检测项目,填补了国内在该项目检测技术上的空白,为今后的相关检测提供技术参考,以更好地应对日益严峻的贸易壁垒,提升我国纺织品质量安全水平和出口竞争力。……
