液相色谱-二极管阵列检测/质谱联用在活性染料结构鉴定中的应用

基于多年运用液相色谱-二极管阵列检测/质谱(HPLC-DAD/MS)联用技术分析活性染料的实验积累,总结了HPLC-DAD/MS联用方法在商品活性染料结构鉴定中的重要应用。商品染料不需要纯化即可通过单次进样达到复杂组分的分离并得到光谱和质谱信息;结合衍生物质量差值法可推定染料的活性基种类和数目;采用二极管阵列检测器的全光谱扫描功能可以得到染料的发色体类别等有用的信息。HPLC-DAD/MS联用方法简便、快速、准确,尤其适用于多组分拼混的商品染料的结构鉴定,有较大的实用价值。通过对多组分商品染料活性灰、活性深黑、海洋蓝中关键组分的结构分析实例,介绍了HPLC-DAD/MS联用分析技术在未知商品活性染料结构分析中的应用。

Structure identification of reactive dyes by high performance liquid chromatography-photodiode array detection/mass spectrometry

Based on years of experience on analyzing reactive dyes by high performance liquid chromatography-photodiode array detection/mass spectrometry (HPLC-DAD/MS), the essential applications for current structure identification of the commercial reactive dyes are summarized in three aspects. Commercial dyes always include several kinds of components. They are assistants for increasing solubility of synthetic dyes, multi-color synthetic dyes and their by-products derived from synthesis and storage. HPLC-DAD/MS technique can separate most of the components, and provide UV-Vis spectra and mass spectra individually. The separation and analysis can be achieved only through one injection without pre-purification of commercial dyes. Compared with traditional analytical methods, HPLC-DAD/MS technique reduces greatly not only the workload of analysis but also provides fully the actual compositions of the dyestuff. The reactive groups can react with ethanolamine or diethanolamine under moderate condition without structure destruction of dyes. The molecular masses before and after derivatization can be determined by MS, and then the type and number of reactive groups can be ascertained by so called "mass difference by derivative method". The chromophore of the dye can be identified by full spectrum scanning function of DAD. HPLC-DAD/MS analytical technique is very special and useful for the structure analysis of multi-component mixed commercial dyes. As examples, the identifications of three multi-component mixed structures of commercial dyes (Reactive Gray, Reactive Supra Black and Reactive Marine Blue) were given.