LC-MS/MS法测定童车纺织品中的3种有机磷阻燃剂

Determination of three phosphate flame retardants in textiles for strollers by LC-MS/MS

建立了液相色谱串联质谱法测定童车用纺织品中3种有机磷阻燃剂的方法,以丙酮为萃取溶剂,超声提取,采用电喷雾正离子源(ESI+)和多反应监测模式(MRM),外标法定量。试验考察了不同流动相对三-(2-氯乙基)磷酸酯(TCEP)、三-(1-氯-2-丙基)磷酸酯(TCPP)和三-(1,3二氯丙基)磷酸酯(TDCP)离子化效率的影响,优化了MRM裂解电压和碰撞能量等参数。结果表明,TCEP、TCPP和TDCP的质量浓度在一定范围内与峰面积呈线性关系,相关系数>0.995,方法检出限0.1 mg/kg,加标回收率在85.0%～114.5%之间,测定值的相对标准偏差(n=6)在4.6%～9.5%之间。该方法前处理简单,定性定量准确,能够满足欧盟对有机磷阻燃剂5 mg/kg的限量要求。

The method of determination of tris（2-chloroethyb phosphate（TCEP）, tris（1-chloro-g-propyb phosphate（TCPP） and tris（1,3-dichloroisopropyl）phosphate （TDCP） in textile for strollers by LC-MS/MS is established. Samples are extracted with acetone under ultrasonic, then are analyzed by LC-MS/MS （ESI＋ and MRM）, external standard for quantitative method. The effect of different mobile phase to ionization efficiency of TCEP ,TCPP and TDCP is researched. The fragment voltage and collission voltage pa- rameters of MRM are optimized. The results show that the mass concentration of TCEP, TCPP and TD- CP is linear with the peak area within a certain range, the correlation coefficient is 〉0.995, the detection limit of the method is 0.1 mg/kg, and the recoveries are between 85.0%-114.5% with 4.6%-9.5% of relative standard deviations （n=6）. The method is simple, accurate, and is suitable for routine analysis of residual phosphate flame retardant in textiles, and meet the EU＇s requirements for the limitation of 5 mg/kg.