Shen Hao-Yu
Analysis and Testing Center, Ningbo Institute of Technology, Zhejiang University, 1st Qianhu Nan Road, Ningbo 315100, Zhejiang, China.
Talanta. 2005 Apr 30;66(3):734-9. doi: 10.1016/j.talanta.2004.12.021. Epub 2005 Jan 6.
Studies on determination of eight kinds of phthalates, e.g. di-ethyl phthalate (DEP), di-propyl phthalate (DPP), di-isobutyl phthalate (DIBP), di-butyl phthalate (DBP), benzyl butyl phthalate (BBP), di-cyclohexyl phthalate (DCHP), di-(2-ethylhexyl) phthalate (DEHP), di-octyl phthalate (DOP), in 25 kinds of plastic products for food use, including packaging bags, packaging film, containers, boxes for microwave oven use, sucking tubes, spoons, cups, plates, etc. by gas chromatography in combination with mass spectrometry detector (GC-MS) in electronic ionisation mode (EI) with selected-ion monitoring (SIM) acquisition method (GC-MS (EI-SIM)) have been carried out. Methods have been developed for both qualitative and quantitative analysis of phthalates. Extraction, clean-up and analysis procedure have been optimized. Determination of samples were performed after frozen in liquid nitrogen and sonication-assisted extraction with hexane, clean-up with LC-C18 SPE and analyzed by GC-MS methods. The base peak (m/z=149) of all the phthalates was selected for the screening studies. The characteristic ions, 121, 177, 222 for DEP; 191, 209 for DPP; 57, 223 for DIBP; 104 for DBP; 91, 132, 206 for BBP; 55, 167 for DCHP; 113, 167, 279 for DEHP; 279 for DOP were chosen for quantitative studies. These techniques are possible to detect phthalates at the level of 10.0mug/kg. Overall recoveries were 82-106% with R.S.D. values at 3.8-10.2%. Only one of the 25 examined samples was free from phthalates. The rest 24 samples were found to contain at least three or more of these phthalates. The predominant phthalate detected in the studied samples was DEHP.
采用气相色谱结合电子轰击电离模式(EI)下的质谱检测器(GC-MS)以及选择离子监测(SIM)采集方法(GC-MS(EI-SIM)),对25种食品用塑料制品(包括包装袋、包装膜、容器、微波炉用盒、吸管、勺子、杯子、盘子等)中的8种邻苯二甲酸酯类物质进行了测定,这些邻苯二甲酸酯类物质包括邻苯二甲酸二乙酯(DEP)、邻苯二甲酸二丙酯(DPP)、邻苯二甲酸二异丁酯(DIBP)、邻苯二甲酸二丁酯(DBP)、邻苯二甲酸苄基丁酯(BBP)、邻苯二甲酸二环己酯(DCHP)、邻苯二甲酸二(2-乙基己基)酯(DEHP)、邻苯二甲酸二辛酯(DOP)。已开发出邻苯二甲酸酯类物质的定性和定量分析方法。对萃取、净化和分析程序进行了优化。样品经液氮冷冻后,用己烷进行超声辅助萃取,通过LC-C18固相萃取柱净化,然后用GC-MS方法进行测定。选择所有邻苯二甲酸酯类物质的基峰(m/z = 149)进行筛查研究。选择DEP的特征离子121、177、222;DPP的191、209;DIBP的57、223;DBP的104;BBP的91、132、206;DCHP的55、167;DEHP的113、167、279;DOP的279进行定量研究。这些技术能够检测出含量低至10.0μg/kg的邻苯二甲酸酯类物质。总体回收率为82% - 106%,相对标准偏差(R.S.D.)为3.8% - 10.2%。在检测的25个样品中,只有1个样品未检出邻苯二甲酸酯类物质。其余24个样品被发现至少含有三种或更多的这些邻苯二甲酸酯类物质。在所研究的样品中检测到的主要邻苯二甲酸酯类物质是DEHP。