液相色谱-串联质谱法对光引发剂异丙基硫杂蒽酮与对-N,N-二甲氨基苯甲酸异辛酯残留量的检测  

Determination of Photoinitators 2-Isopropyl Thioxanthone and 2-Ethylhexyl-4-dimethylaminobenzoate Residues by Liquid Chromatography Coupled to Tandem Mass Spectrometry

作　　者：生茂强[1] 邓晓军[2] 郭德华[2] 陈舜胜[1] 

机构地区：[1]上海海洋大学食品学院,上海200090 [2]上海出入境检验检疫局,上海200135

出　　处：《分析测试学报》2009年第1期12-17,21,共7页Journal of Instrumental Analysis

基　　金：上海市应对技术性贸易专项基金资助项目(06TBT09)

摘　　要：建立了液相色谱-串联质谱法检测饮料中光引发剂异丙基硫杂蒽酮(ITX)及其协同试剂对-N,N-二甲氨基苯甲酸异辛酯(EHDAB)残留量的测定方法。使用D7-ITX为内标,样品经Carrez试剂沉淀蛋白质后用乙腈-水(体积比60:40)提取,上层提取液用HLB固相萃取柱净化。采用多反应监测(MRM)正离子模式检测,定性离子对为m/z255>213,m/z255>184(ITX)和m/z278>166,m/z278>151(EHDAB),采用m/z255>213和m/z278>166进行定量。实验结果表明,ITX和EHDAB的定量下限均为0.1μg/kg,ITX在0.2～20μg/kg范围内线性相关系数为0.9997;EHDAB在0.1～10μg/kg范围内线性相关系数为0.9998。牛奶、果汁和奶酪3种基质中添加0.5、1.0、2.0μg/kg3个水平的回收率为87%～119%,相对标准偏差为2.5%～9.5%,满足对饮料中ITX和EHDAB的检测需求。This paper presented a liquid chromatography - tandem mass spectrometry （ LC - MS/MS） method for determination of photoinitiators 2-isopropyl thioxanthone（ITX） and its synergistic agent 2- ethylhexyl-4-dimethylaminobenzoate（EHDAB） residues in beverage and food. The sample was precipitated and extracted by using aeetonitrile water（60 ： 40, by volume） containing Carrez reagent. The supernatant was cleaned up by HLB solid phase extraction cartridge. Residues were detected by MS/MS technique using positive electrospray ionization and multiple reaction monitoring （MRM） mode, and employing two precursor- product ion pairs： m/z 255 〉213, m/z 255 〉 184（ITX） and m/z 278 〉 166, m/z 278 〉 151 （EHDAB） as qualitative ion pairs, and m/z 255 〉 213, and m/z 278 〉 166 as quantification ion pairs. DT-ITX was used as an internal standard. The result showed that the quantitation limits of ITX and EHDAB were both 0. 1 μg/kg. The calibration curves showed good linearity for ITX and EHDAB in the ranges of 0. 2 -20 μg/kg and 0. 1 - 10μg/kg, respectively, and the correlative coefficient were O. 999 7 and 0. 999 8, respectively. The average recoveries from three matrices of milk, beverage and cheese spiked at three levels of 0. 5, 1.0, 2.0 μg/kg were between 87% and 119% with RSD（n =6） of 2.5%- 9.5% . The method was reliable and sen- sitive for daily inspection of ITX and EHDAB residues in beverage and food.

关 键 词：异丙基硫杂蒽酮 对-N N-二甲氨基苯甲酸异辛酯 液相色谱-质谱 残留 

分 类 号：O657.63[理学—分析化学] TS272.7[理学—化学]