Synthesis And Application Of Derivatization Reagents For The Analysis Of Carboxylic Acids And Amines

The derivatization technique in analytical chemistry is to make the components to be tested in the sample a derivative,making it more suitable for a particular analytical method.The role of derivatization in chromatographic analysis is summarized as follows:(1)to improve the detection sensitivity of the test object;(2)to change the chromatographic properties of the compound to improve the separation effect;(3)suitable for further identification of compounds;(4)to expand the application of chromatographic analysis.In this paper,the development and utilization of carboxylic acid and amine derivatives were studied.The main research contents are as follows:1.Application of derivatization reagent APy-PPZ((S)-1-[3-(4-methylpiperazine)-4,6-dinitro-phenyl]-3-aminopyrrolidine).Ketoprofen(KET)was used as the research object,and its analysis was carried out.In this experiment,the separation of enantiomers of KET and the content of ketoprofen in the drug were detected by column pre-column derivatization-high performance liquid chromatography(HPLC).Finally,the content of ketoprofen was successfully detected.And then,in this paper,the stable isotope labeling method was established,and the content of ketoprofen in saliva was analyzed by LC-ESI-MS.So in the acidic mobile phase conditions,ketoprofen was first separated by HPLC,and then was detected in the positive ion mode ESI-MS,in which can get high ionization efficiency and the corresponding high detection sensitivity.Using this method,we successfully detected the content of ketoprofen in saliva after 3 hours of taking the drug.The content of S-ketoprofen was 2.26 ng/mL,and the content of R-ketoprofen was 1.1 ng/ML.2.Synthesis of stabilized isotope labeling reagent 1-(2,4-dinitro-5-fluorophenyl)-4,4-dimethylpiperazinium iodide(MPPZ)In recent years,the LC-MS method has been developed rapidly,and has become the mainstream technology of protein group quantitative.In view of the fact that the first-order mass spectrometry labeling method is difficult to achieve at the same time more than four markers,we designed a five-labeled reagent.In this paper,the stable isotope labeling reagent MPPZ was synthesized.Synthesis method:1-(2,4-dinitro-5-fluorophenyl)-4-methylpiperazine directly react with iodomethane at 60 ? for 30 min to get MPPZ.