Synthesis And Chiral Resolution Of 2,3-Dihydroxy Succinate Derivatives

Chirality is one of the basic attributes of nature.Most drugs,whether natural or synthetic,have a chiral structure.Chiral drug enantiomers,though chemically identical,may produce completely opposite pharmacological effects.Therefore,the structures of finished drugs and news under development are essential to be analyzed.Chromatography as the most commonly used method for chiral drug analysis,which uses chiral resolution reagents to separate drugs,is efficient and rapidly.The mature additives that have been used are cyclodextrins and their derivatives,proteins,crown ethers,metal complexes and antibiotics.In this dissertation,two chiral resolving agents with chiral resolution were prepared by simple esterification,and three chiral drugs with ultraviolet absorption and five without were used to test the chiral separation.Performance.By determining the composition,concentration,and p H of the running buffer,the optimal resolution conditions were determined.The main research contents are as follows:(1)Polysorbitol tartarate was synthesized using tartaric acid and sorbitol,which has good water solubility.It has good compatibility and is not easily precipitated in capillary electrophoresis running buffer.It can be storaged for a long time due to the stable properties.Mild,convenient post-treatment,simple operation,high yield.The chiral recognitioneffectcanbeenhanced,becausethesynthesized polysorbitol tartarate has a molecular weight of more than 10~3,which has multiple chiral C atoms and hydroxyl groups.It was found that sorbitan tartrate has a stable UV absorption between 200 nm and 220nm,and can be used as a UV absorbing background to directly detect chiral drugs without UV absorption.The results showed that the eight chiral drugs showed signs of separation under different separation conditions.(2)Usesd tartaric acid and lactic acid to synthesize Polylactate tartarate,the polymer has high viscosity,good water solubility and stable properties.At the same time,the experimental conditions are mild,the post-processing is convenient,the yield is high,and the operation is simple.The synthesized polylactate tartarate has a molecular weight over 10~4,which contains a plurality of chiral C atoms and hydroxyl groups.It enhances the water solubility and chiral recognition effect of the polymer.It has been found that polylactate tartarate also has stable UV absorption between 200 nm and 220 nm,and can be directly used as a UV-absorptive background to detect non-UV-absorbing chiral drugs.The results show that the six chiral drugs were separated under different conditions.(3)Establishing a capillary electrophoresis analysis method to detect the ADP,HYP,IMP,INO nucleotides in pork.Using the simplest capillary zone electrophoresis-ultraviolet detector,through the optimization of conditions and methodological investigation,the optimal analytical conditions were determined as follows:12 mmol/L borax(p H10.0)was used as running buffer solution,and the separation voltage was 25 k V.The detection wavelength was 214nm and the capillary temperature was 25°C.Four nucleotides were effectively separated in 13 minutes.The minimum detectable limit of four nucleotides was 0.40 mg/L,the precision was 1.29-10.8%during the day,and the intraday precision was 0.37-3.97%.The recovery of four nucleotides in actual pork samples was spiked.103.69-107.09%with a linear range of 20-100 mg/L.The method is simple,rapid in analysis,and low in detection limit,which can provide reference for nucleotide detection in pork samples.