高效液相色谱法测定聚苯乙烯发泡塑料中防老剂2246的含量  

HPLC Determination of Antioxidant 2246 in Polystyrene Foamed Plastics

作　　者：王乐[1] 王飞[1] 陈晞[1] 张爱霞[1] 郑新华[1] 陶琳[2] 

机构地区：[1]济南出入境检验检疫局,济南250014 [2]淄博出入境检验检疫局,淄博255031

出　　处：《理化检验（化学分册）》2017年第1期50-54,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：质检总局科研项目(2015IK212;2014IK266)

摘　　要：将样品0.250 0g溶于乙酸乙酯5mL中,加甲醇15mL使聚合物沉淀,静置5min,将上清液取出留用。沉淀用甲醇(每次5mL)超声洗涤3次,所得洗液与上清液合并,用甲醇定量稀释至50mL作为待测液供色谱分析。以Agela Venusil XBP C18色谱柱为固定相,以甲醇(9+1)溶液为流动相进行分离,外标法定量。防老剂2246的质量浓度在0.100~10.0mg·L-1范围内与相应的色谱峰面积呈线性关系。方法的测定下限(10S/N)为0.002%。在2个浓度水平(0.100%,0.250%)上进行加标回收试验,测得回收率依次为99.8%,97.7%,测定值的相对标准偏差(n=6)依次为0.3%,0.2%。色谱法测定结果经高效液相色谱-串联质谱法作进一步确证。The sample 0. 250 0 g was dissolved in 5 mL of ethyl acetate, and contents of polymers in the solution were precipitated by addition of 15 mL of methanol. After standing for 5 rain, the supernatant was taken and preserved. The precipitate was washed ultrasonically with methanol （5 mL in each washing） for 3 times. The washings were combined with the sepernatant and diluted to 50. 0 mL with methanol. The solution was used for HPLC determination of the antioxidant 2246, using the column of Agela Venusil XBP C18 as the stationary phase and mixture of CH3OH and H20 （9 ＋ 1） as mobile phase in the separation. Method of external standard was adopted for quantification, Linear relationship between values of peak area and the respective mass concentrations of the antioxidant 2246 was kept in the range of 0. 100 - 10. 0 mg · L^-1 , and value of lower limit of determination （10S/N） was found to be 0. 002%. Test for recovery was made by addition of standard solution at 2 concentration levels of 0. 100%, 0, 250%, giving values of recovery of 99. 8%, 97. 7% and RSDs （n=6） of 0. 3%, 0. 2% respectively. The results of HPLC were further verified by HPLC-MS/MS analysis.

关 键 词：高效液相色谱法 聚苯乙烯发泡塑料 防老剂2246 高效液相色谱-串联质谱法 

分 类 号：O652.63[理学—分析化学]