高效液相色谱-串联电感耦合等离子体质谱法测定塑料中3种溴化阻燃剂

Determination of Bromine Flame Retardants in Polymers by High Performance Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry

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.