Analysis Of Drug Related Substances And Urinary Modified Nucleosides By LC/MS Technology

The application field of LC/ESI-MS is very wide.80% of the organic compounds can be separated by liquid chromatogram and the ESI can produces multiply charged ions, then LC/MS technology became to be used in analysis of some very new compounds. For the advantages of high efficiency of separation, exceptional speed of analysis, high sensitivity and high resolution, LC/MS has become more sample in pretreatment and separation of the complex mixture and it's a very important characteristic of LC/MS to analysis the trace compounds from biological product.In this dissertation, the fundamental, development situation and applied range of LC/MS are summarized and two respects content are introduced. First, clindamycin-2-phosphate and cinepazide maleate was determined and quantitated by HPLC/ESI/QTOF/MS, second, the modified nucleoside of urine from patients with bladder cancer were quantitated. Specific research contents and results are as follows:1. The new standard lincomycin-2-phosphate has been synthetized and its fragmentation pathways have been analyzed. The four major impurities of clindamycin-2-phosphate injection have been quantitated and the major impurities of six different injections were quantitated and compared by HPLC/ESI/QTOF/MS.2. HPLC/ESI/QTOF/MS method for separation and characteration of related substances of cinepazide maleate has been established at the first time and it is convenience, fast and accuracy in use of determining Z/E cinepazide maleate.3. We detected 22 modified nucleosides from 50 bladder cancer patients and 16 normal persons, then all of the 22 modified nucleosides were quantiteted. ROC curve of the modified nucleoside content were prepared by SPSS16.0 software. From the ROC curve, we analysis the sensitivity and specificity of the modified nucleoside for the diagnosis of bladder cancer. It turned out that five of the modified nucleosides have diagnostic value.