Rothenbacher Thorsten, Schwack Wolfgang
Institut für Lebensmittelchemie, Universität Hohenheim, Garbenstr. 28, 70599 Stuttgart, Germany.
Rapid Commun Mass Spectrom. 2009 Sep;23(17):2829-35. doi: 10.1002/rcm.4194.
In the European Community, selected phthalic acid esters (PAE) are restricted in their use for the manufacture of toys and childcare articles to a content of 0.1% by weight. As PAE are mainly used as plasticisers for poly(vinyl chloride) (PVC), a rapid screening method for PVC samples with direct analysis in real time ionisation and single-quadrupole mass spectrometry (DART-MS) was developed. Using the ions for the protonated molecules, a limit of detection (LOD) of 0.05% was obtained for benzyl butyl phthalate, bis(2-ethylhexyl) phthalate and diisononyl phthalate, while for dibutyl phthalate, di-n-octyl phthalate and diisodecyl phthalate the LOD was 0.1%. Validation of identification by the presence of ammonium adducts and characteristic fragment ions was possible to a content of >or=1% for all PAE, except for benzyl butyl phthalate (>or=5%). Based on the fragment ions, bis(2-ethylhexyl) phthalate could clearly be distinguished from di-n-octyl phthalate, if the concentrations were >r=5% and >or=1% at measured DART helium temperatures of 130 and 310 degrees C, respectively. The complete analysis of one sample only took about 8 min. At the generally used gas temperature of 130 degrees C, most toy and childcare samples did not sustain damage if their shape fitted into the DART source.
在欧洲共同体，特定邻苯二甲酸酯（PAE）在玩具和儿童护理用品制造中的使用限制为重量含量0.1%。由于PAE主要用作聚氯乙烯（PVC）的增塑剂，因此开发了一种用于PVC样品的快速筛选方法，即实时电离和单四极杆质谱直接分析（DART-MS）。利用质子化分子的离子，邻苯二甲酸苄基丁酯、邻苯二甲酸二（2-乙基己基）酯和邻苯二甲酸二异壬酯的检测限（LOD）为0.05%，而邻苯二甲酸二丁酯、邻苯二甲酸二正辛酯和邻苯二甲酸二异癸酯的LOD为0.1%。除邻苯二甲酸苄基丁酯（≥5%）外，所有PAE在铵加合物和特征碎片离子存在下进行鉴定的验证含量≥1%时均可行。基于碎片离子，在测量的DART氦气温度分别为130和310℃时，如果浓度≥5%和≥1%，邻苯二甲酸二（2-乙基己基）酯可以与邻苯二甲酸二正辛酯明显区分。分析一个样品仅需约8分钟。在通常使用的130℃气体温度下，如果玩具和儿童护理样品的形状适合放入DART源中，大多数样品不会受到损坏。
