Institute of Industrial and Consumer Product Safety, Chinese Academy of Inspection and Quarantine, Beijing, China.
J Sep Sci. 2018 Feb;41(3):657-668. doi: 10.1002/jssc.201700556. Epub 2017 Dec 14.
This paper presents a simple, rapid, and green method based on a static headspace gas chromatography-mass spectrometry for determining 58 fragrance allergens in plush toys. This study is the first to meet the requirement for simultaneously determining 66 fragrances, except for eight natural extracts restricted by the European Toy Safety Directive 2009/48/EC. A minimal amount of sample (20 mg) and acetone solvent (20 μL) were placed in a headspace vial. A gas-solid equilibration of fragrances between the headspace and the sample was achieved within 10 min under the vapor atmosphere of acetone at 200°C, which allowed the fragrances in the sample to be measured by gas chromatography-mass spectrometry. Results showed that the interference caused by different sample matrices was negligible. The proposed method exhibited determination results that were highly similar to those of traditional ultrasonic extraction with sufficient sensitivity (limits of quantification: 0.02-10 mg/kg) for 58 fragrances, indicating its accuracy and reliability. The average recoveries ranged from 71.3 to 137.4%, and the relative standard deviation (n = 6) varied from 1.1 to 18.0%. Finally, the method was applied to monitor the fragrances in 20 commercial toys. This study provides a good reference for rapidly and greenly determining the semi-volatile analytes in toys, textiles, and other products.
本文提出了一种基于静态顶空气相色谱-质谱联用的简单、快速、绿色的方法,用于测定毛绒玩具中的 58 种香料过敏原。本研究首次满足了同时测定 66 种香料的要求,除了欧洲玩具安全指令 2009/48/EC 限制的八种天然提取物外。只需少量样品(20mg)和丙酮溶剂(20μL),即可将其置于顶空瓶中。在 200°C 的丙酮蒸气气氛下,顶空和样品之间的香气在 10min 内达到气固平衡,从而可以通过气相色谱-质谱法测定样品中的香气。结果表明,不同样品基质引起的干扰可以忽略不计。该方法与传统超声提取法具有高度相似的测定结果,灵敏度高(定量限:0.02-10mg/kg),适用于 58 种香料,表明其准确性和可靠性。平均回收率在 71.3%至 137.4%之间,相对标准偏差(n=6)在 1.1%至 18.0%之间。最后,该方法应用于监测 20 种商业玩具中的香料。本研究为快速、绿色地测定玩具、纺织品和其他产品中的半挥发性分析物提供了良好的参考。