Ohgaki Masataka, Takeguchi Yuko, Okawa Shin, Namiki Kenji
Hitachi High-Tech Science Corporation, Shintomi 2-15-5, Chuo-ku, Tokyo 104-0041, Japan.
R Soc Open Sci. 2019 Feb 27;6(2):181469. doi: 10.1098/rsos.181469. eCollection 2019 Feb.
In 2013, the European Union expanded the list of hazardous substances contained in the RoHS Directive. In addition, certain phthalate esters, such as dibutyl phthalate (DBP), butyl benzyl phthalate (BBP), di-2-ethylhexyl phthalate (DEHP) and diisobutyl phthalate (DIBP), will be categorized as RoHS-prohibited substances starting from July 2019. Although pyrolysis-gas chromatography-mass spectrometry (Py-GC-MS) is a promising analytical method for the screening of phthalate esters, we have developed a novel soft-ionization MS method that is quantitative as well as faster and more convenient for this purpose. The sample was measured three times, after providing the calibration curve using a powdery standard material of SPEX. The data collection time is 5 min, and continuous measurements are completed within 8 min per sample. The mass spectrum was corrected by dividing the intensity by the sample weight. For the coefficient of variation, DBP was 2.9%, BBP was 3.4%, DEHP was 3.6%, and good reproducibility was observed. Precise analyses of phthalate esters using traditional methods can require solvent extraction times of up to 24 h as well as special techniques. Therefore, a screening method that can be easily carried out by anyone within ten minutes is very attractive.
2013年，欧盟扩大了《限制有害物质指令》（RoHS指令）中所含有害物质的清单。此外，某些邻苯二甲酸酯，如邻苯二甲酸二丁酯（DBP）、邻苯二甲酸丁苄酯（BBP）、邻苯二甲酸二（2-乙基己基）酯（DEHP）和邻苯二甲酸二异丁酯（DIBP），自2019年7月起将被归类为RoHS指令禁止的物质。尽管热解气相色谱-质谱联用（Py-GC-MS）是一种很有前景的邻苯二甲酸酯筛选分析方法，但我们开发了一种新型软电离质谱方法，该方法具有定量功能，且为此目的更快、更方便。使用SPEX的粉末标准物质提供校准曲线后，对样品进行了三次测量。数据采集时间为5分钟，每个样品在8分钟内完成连续测量。通过将强度除以样品重量对质谱进行校正。对于变异系数，DBP为2.9%，BBP为3.4%，DEHP为3.6%，观察到良好的重现性。使用传统方法对邻苯二甲酸酯进行精确分析可能需要长达24小时的溶剂萃取时间以及特殊技术。因此，一种任何人都能在十分钟内轻松完成的筛选方法非常有吸引力。
