HPLC-MS/MS联用技术定性定量分析

通过MS/MS技术定性检测，证明环己酮生产的副产物主要成分为己二酸、戊二酸、丁二酸及其脱水产物。以40%甲醇和60％水（用甲酸调节pH值至3.5）作为流动相，经Hypersil GOLD C₁₈ 色谱柱初步分离，利用串联质谱选择反应离子监测(SRM)方式监测己二酸、戊二酸、丁二酸的负离子，进行外标法定量测定。结果表明，己二酸在32～600 μg•kg^-1、戊二酸在8～150 μg•kg^-1、丁二酸在8～150 μg•kg^-1的浓度范围内线性关系良好，线性相关系数均大于0.995 0。用此方法检测环己酮实际生产过程中的副产物，己二酸、戊二酸、丁二酸的质量百分含量分别为80.140％、7.316％和6.170％，相对标准偏差均小于8％。

Qualitative and Quantitative Analysis of the By-Products in the Course of Cyclohexone Production by HPLC-MS/MS

Methods of qualitative and quantitative analysis of the by-product in the course of cyclohexone production were established by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Firstly, the variety involved in the sample was tested quantitative by MS/MS, of which the main components were adipic acid, pentanedioic acid, butanedioic acid and the products of their dehydration. The sample was seperated on Hypersil GOLD C₁₈ with 40% methanol and 60% water (pH was tuned up to 3.5 by formic acid) as the mobile phase. Detection was performed on a tandem mass spectrometry in selective reaction monitoring (SRM) mode. Then peak areas were quantitated. The results indicate that the linear range of adipic acid, pentanedioic acid and butanedioic acid are 32-600 μg•kg^-1, 8-150 μg•kg^-1, 8-150 μg•kg^-1 respectively with correlation coefficients of all stadard curves more than 0.995 0. The content of adipic acid, pentanedioic acid and butanedioic acid in the sample are 80.140%, 7.316% and 6.170% respectively with relative standard deviation of all samples less than 8％. This method is sensitive, accurate and will be apply to the determination of adipic acid, pentanedioic acid and butanedioic acid.