高效液相色谱-串联质谱法测定纸质包装材料中米氏酮、对二甲氨基二苯甲酮及2-异丙基硫杂蒽酮的迁移量

摘要

为测定纸质包装材料中米氏酮、对二甲氨基二苯甲酮及2-异丙基硫杂蒽酮的迁移量,建立了磁固相萃取-高效液相色谱-串联质谱检测法(MSPE-HPLC-MS/MS).该方法采用溶剂热还原法制备了Fe3O4磁性亚微米粒子,以其为固相萃取材料,并以Agilent Eclipse AAA柱为分析柱,甲醇和水溶液为流动相,正离子模式下测定,流量为0.5 mL/min.对磁固相萃取中影响米氏酮、对二甲氨基二苯甲酮及2-异丙基硫杂蒽酮的主要萃取因素(包括磁性纳米粒子用量、洗脱溶剂和体积、PH值)进行了考察.结果表明:米氏酮等3种物质在0.5 ～50 ng/mL范围内线性关系良好(r＞0.999),最低定量限均为0.5 ng/mL,检测限为0.2 ng/mL,3种物质的添加回收率为78.3～92.1％,相对标准偏差小于7.4％,所建立的方法简单、快速、灵敏度高,适用于纸质包装材料中米氏酮、对二甲氨基二苯甲酮及2-异丙基硫杂蒽酮在实际样品中的残留分析检测.%In this manuscript, a magnate solid phase extraction -high performance liquid chromatography -tandem mass spectrometry (MSPE-HPLC-MS/MS) method was established to determine the migration of 4,4' -Bis (dimethylamine) benzophenone,4 -(Dimethy lamino) benzophenone, 2 -Isopropythioxanthone from paper package. The analytes was separated on anrnAgilent Eclipse AAA C18 column with a mobile phase of methanol-water in gradient elution mode at the flow rate of 0.5 mI7min,the mass spectrometry worked in positive ion mode. Moreover, the extraction parameters which affect efficiency were optimized and the results demonstrated that a good linearity in the concentration range of 0.5～50.0 ng/mL for 3 analytes. The correlation coefficients were all higher than 0.999. Average recoveries of 3 analytes at three spiked level ranged from 78.3 to 92.1 %,with RSDs less than 7.4 %. The limits of quantification and detection of the method was 0.5 and 0.2 ng/mL,respectively. The method was proven to be sensitive and simple,and was suitable for the rapid determination the real migration of 4,4' -Bis (dimethylamine) benzophenone,4-(Dimethy lamino) benzophenone,2-Isopropythioxanthone from paper package.