基于高分辨质谱的化妆品中防腐剂类致敏成分高通量检测方法的建立及应用

Establishment and application of high-throughput detection method for preservative allergenic ingredients in cosmetics based on obitrap high resolution mass spectrometry

中文关键词:  静电场轨道阱高分辨质谱法  化妆品  致敏成分  高通量检测

英文关键词:obitrap high-resolution mass spectrometry  cosmetics  allergenic ingredients  high-throughput analysis

中文摘要:

      目的 基于静电场轨道阱高分辨质谱, 建立化妆品中异噻唑啉酮类、甲醛释放剂、对羟基苯甲酸酯类、酸类4大类防腐剂类致敏成分的高通量检测方法, 并应用于实际样品中致敏成分的筛查与定量分析。方法 利用致敏成分标准品通过高分辨质谱正负离子切换FullMS/ddMS2扫描方式分析, 获得多种致敏成分的保留时间、一级母离子和二级碎片离子精确质量数, 构建致敏成分筛查谱库。样品经50%甲醇水溶液超声提取后, 经ZORBAX Eclipse Plus C18 (3.0 mm×100 mm, 1.8 μm)色谱柱分离, 采用高分辨质谱分析, 利用TraceFinder软件对化妆品中致敏成分与谱库相关信息匹配, 实现目标物的高通量筛查确证, 筛查确认后利用一级母离子外标法进行致敏成分的定量分析。结果 筛查方法既有一级母离子精确质量数和保留时间, 又有二级碎片离子信息, 其筛查确证结果可靠; 目标化合物在相应的质量浓度范围内线性关系良好(r2>0.99), 检出限为0.2~20 μg/g, 回收率为85.6%~109.7%, 相对标准偏差为3.2%~12.8%, 能够满足检测需求。结论 该方法简单、准确、快速, 可用于化妆品中多种致敏成分的高通量快速筛查和定量分析。

英文摘要:

      Objective To establish a high throughput detection method for 4 kinds of preservative allergenic ingredients in cosmetics based on obitrap high resolution mass spectrometry and apply it for the screening and quantitative analysis of sensitizing ingredients in practical samples. Methods The retention time, accurate mass numbers of primary and secondary fragment ions for various allergenic ingredients were obtained from standard solution by high resolution mass spectrometry with positive and negative ion switching FullMS/ddMS2 scanning mode, and the screening library of sensitizing components were established. The samples were extracted with 50% methanol solution, separated by ZORBAX Eclipse Plus C18 column (3.0 mm×100 mm, 1.8 μm), analyzed by high-resolution mass spectrometry, and confirmed by high-throughput screening by matching the information of allergenic ingredients in the screening library with TraceFinder software. Quantitative analysis of sensitizing components was carried out by parent ions external standard method after screening and confirmation. Results The screening method had both the accurate mass and retention time of the primary parent ion and the seondary fragment ion information. The results of screening allergenic ingredients were reliable. The target compound had a good linear relationship within the corresponding mass concentration range (r2>0.99). The limits of detection of this method were 0.2?20 μg/g. The recoveries were in the range of 85.6%?109.7% and the relative standard deviations were 3.2%?12.8%, which could meet the detection requirements. Conclusion This method is simple, sensitive, accurate and suitable for the rapid screening and confirmation of a variety of preservative allergenic ingredients in cosmetics.