建立了塑料中十溴联苯醚(BDE209)、十溴联苯(BB209)和六溴苯(HBB)3种溴化阻燃剂(BFRs)的高效液相色谱串联电感耦合等离子体质谱(HPLC-ICP-MS)定量测定方法。采用AgilentTC-C18色谱柱(250mm×4.6mm,5μm)分离,异丙醇-甲醇-水(60:30:10,V/V)为流动相等度洗脱,流速为0.8mL/min。聚乙烯(PE)、丙烯腈-丁二烯-苯乙烯共聚物(ABS)和聚苯乙烯(PS)3种塑料样品均采用甲苯超声辅助提取、异辛烷和甲醇进一步沉淀净化的方法进行样品前处理。实验优化了液相色谱分离条件和质谱参数、考察了PE、ABS和PS的基质效应。方法的线性范围0.25~10mg/L,线性相关系数r〉0.9999,加标回收率75.7%~108.7%,3种化合物的仪器的检出限(LOD,S/N=3)和定量限(LOQ,S/N=10)分别为0.097~0.1mg/L和0.243~0.250mg/L。PE,ABS和PS基体对HBB,PBB209和PBDE209响应的抑制在25%,10%和3%左右,说明基质成分对准确定量有较大影响。结果表明,方法简便、专属性强、灵敏度高,适用于塑料样品中溴化阻燃剂的定量分析。
A study was performed to determine decabromodiphenyl ether (BDE209), decabromobiphenyl (BB209) and hexabromobenzene(HBB) in polymers by high performance liquid chromatography-inductively coupled plasma mass spectrometry(HPLC4CP-MS). Agilent TC-Cls column(250 mm×4.6 ram, 5 μm) was used with isopropanol/methanol/water (60: 30: 10, V/V) as mobile phase at flow rate of 0. 8 mL/min. Samples were extracted with toluene, using ultrasonic-assisted extraction ( UAE), and then precipitated by isooctane and methanol. Chromatographic separation and mass spectrometric conditions were optimized, and matrix effect of polystyrene ( PS), acrylonitrile-butadiene-styrene copolymer (ABS) and polyethylene (PE) were evaluated . The calibration curve was linear within the range from 0.25 mg/L to 10 mg/L with a correlation coefficient of 0. 9999. The recoveries of addition standard were in the range of 75.9% -103.8%. The LOD (S/N=3) and the LOQ (S/N= 10) were within the range of 0. 097-0. 1 mg/L and 0. 243- 0. 250 mg/L. The matrix inhibitions of HBB, BB209 and BDE209 in PE, ABS and PS were 25%, 10% and 3%, respectively. The results proved that the method is simple, selective, specific and suitable for determination of bromine flame retardants in polymers.