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

Simultaneous Determination the Migration of 4,4’-Bis(Dimethylamine) Benzophenone, 4-(Dimethy Lamino) Benzophenone and 2-Isopropythioxanthone from Paper Package by Magnate Solid Phase Extraction-High Performance Liquid Chromatography-Tandem Mass Spectrometr

DOI：10.3969/j.issn.1673-1689.2012.11.007

中文关键词: 磁性亚微米粒子 米氏酮 对二甲氨基二苯甲酮 2-异丙基硫杂蒽酮 纸质包装材料

英文关键词: micro-disperse ferrite microspheres 4 4’-Bis(dimethylamine) benzophenone 4(Dimethy lamino) benzophenone 2-Isopropythioxanthone paper package

基金项目:国家“十一五”科技支撑计划项目(2011BAK10B05,2012BAD29B05)

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中文摘要:

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。

英文摘要:

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 an Agilent Eclipse AAA C18 column with a mobile phase of methanol-water in gradient elution mode at the flow rate of 0.5 mL/min,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.

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