固相萃取结合气相色谱-质谱法测定皮革中的14种阻燃剂  

Determination of 14 Kinds of Flame Retardants in Leather by Solid Phase Extraction Combined with GC-MS Method

作　　者：王莉[1] 王斌[1] 罗海英[1] 冼燕萍[1] 吴玉銮[1] 董浩[1] 陈宗良[1] 

机构地区：[1]广州质量监督检测研究院国家皮革制品质量监督检验中心(广州),广东广州511447

出　　处：《分析测试学报》2016年第12期1548-1553,共6页Journal of Instrumental Analysis

基　　金：广东省质量技术监督局科技项目(2015PZ06);广州市质量技术监督局科技项目(2014KJ37)

摘　　要：采用固相萃取结合气相色谱-质谱（GC-MS）技术,建立了皮革中14种多氯联苯及磷酸三酯类阻燃剂（TEP,TBP,TCEP,PCB18,TCPP,PCB101,PCB153,PCB138,TPh P,TEHP,PCB180,o-TTP,m-TTP,p-TTP）的高通量检测方法。皮革样品经乙腈超声提取后,采用Florisil固相萃取柱净化,经DB-5MS色谱柱分离,GC-MS的选择离子监测（SIM）模式监测,以保留时间和特征离子比值定性,外标法定量。14种阻燃剂在一定浓度范围内线性关系良好,相关系数（r2）均大于0.998,方法检出限为25.0-50.0μg/kg,平均回收率为82.0%-112.8%,相对标准偏差（RSD,n=6）为2.1%-9.4%。方法的前处理简单快速,灵敏度高,适用于皮革中14种阻燃剂的同时测定。A new method was established to determine 14 kinds of polychlorinated biphenyls（PCBs） and organophosphate esters（OPEs） flame retardants（ including TEP, TBP, TCEP, PCB18, TCPP, PCB101, PCB153, PCB138, TPhP, TEHP, PCB180, o-TTP, m-TTP and p-TTP） in leather by solid phase extraction（SPE） coupled with gas chromatography - mass spectrometry （ GC - MS）. The samples were ultrasonically extracted with acetonitrile, and purified with a Florisil solid phase extrac- ting column. Analytes were successfully separated on a DB -5MS capillary column, and detected by GC -MS in selected ion monitoring mode （SIM）. Analytes were qualitatively analyzed via retention time and abundance ratio of characteristic ions, and quantified by the external standard method. 14 flame retardants presented favorable linearity in the respective linear ranges, with correlation coeffi- cients（r2） more than 0. 998. The detection limits（ S/N= 3 ） ranged from 25.0 μg/kg to 50. 0 μg/ kg, the average recoveries（n = 6） were in the range of 82.0% - 112. 8% , and the relative standard deviations（RSDs, n =6） were 2. 1% -9.4% . The method is accurate, rapid and sensitive, and is suitable for the determination of 14 flame retardants in leather samples.

关 键 词：皮革 阻燃剂 固相萃取 气相色谱-质谱 

分 类 号：O657.63[理学—分析化学] TQ314.248[理学—化学]