| This thesis mainly research on the application of new organic polymer monolith column on the separation and detection of various natural medicines by capillary electrochromatography methods. Different types of capillary electrochromatography organic polymer monolith columns were prepared and characterized, and applied to the analysis of various types of drugs. A series of practical method for the analysis of natural medicine were also established.The thesis was divided into four parts, including seven chapters. The first part is the Chapter 1, which mainly described the basic theory and development history of capillary electrochromatography, the overall classification of the monolithic columns and the status of their applications in various areas of separation and analysis.In the second part (Chapter 2 and 3), two different types of organic polymer monolith column were prepared and evaluated. In Chapter 2, based on the neutral monomer HEMA and polar crosslinker MBAA, a hydrophilic poly(HEMA-co-MBAA) organic polymer monolith was prepared by in situ free radical polymerization method. The hydroxyl and amino groups on the surface of the monolithic stationary phase provided the polar sites for the hydrophilic interaction. The effects of the composition of the copolymerization mixture and the proportion of each component on the preparation were investigated in detail. The monolithic columns showed good mechanical stability and reproducibility. And the monolithic column was successfully applied to the separation of amines, nucleosides and narcotics. In Chapter 3, a ternary crosslinker was used for the preparation of a hydrophobic poly(BMA-co-TMPTMA) organic polymer monolithic column, and a variety of preparation conditions were optimized. The stationary phase of the monolithic column contained hydrophobic benzyl functional groups and sulfonic acid groups which can produce strong EOF. Fast separation and determination of six alkaloids was achieved based on the monolithic column.In the third part (Chapter 4 and 5), the pCEC-ESI-MS analysis of drugs based on laboratory-made organic polymer monolith column was studied. In Chapter 4, a pCEC-ESI-MS method based on poly(HEMA-co-MBAA) monolithic column for the separation and detection of Belladonna alkaloids was developed for the first time. The method was fast, efficient, sensitive, with good reproducibility and stability. Under optimal conditions, four Belladonna alkaloids can achieve good separation in 7 minutes. The detection limit of the method was 0.05 μg/mL, and the method was successfully applied to the analysis of the actual spiked urine samples. In Chapter 5, we constructed a pCEC-ESI-MS method based on poly(1-hexadecene-co-TMPTMA) monolithic column for the separation and detection of narcotics and β2-agonists for the first time. Three narcotics and two β2-agonists could obtained good baseline separation within 15 minutes under optimal conditions. The detection limit of the established method was 0.09 μg/mL, and the reproducibility was good, with the RSDs (n=5) of retention times and peak areas less than 0.89% and 6.47%, respectively. The method was successfully applied to the analysis of real urine sample form a volunteer who oral took salbutamol sulphate drug.In the fourth part (Chapter 6 and 7), researches on the application of capillary electrophoresis method were carried out. In Chapter 6, a polarity transition online enrichment-microemulsion electrokinetic chromatography method for the simultaneous separation and detection of ten organic acids was performed. The method was applied on the detection of cinnamic acid in the methanol solution of cinnamon bark and protocatechualdehyde in salvia, respectively. In Chapter 7, we established a pseudo-stationary phase micellar electrokinetic chromatography based on a homemade amphiphilic poly(BMA-co-MAA) polymer for the separation and determination of five plant hormones. The method was rapid, sensitive, reproducible, and was applied for the separation of five plant hormones within 14 min. The method was also applied to the determination of naphthaleneacetic acid in the aqueous solution of rooting powder. |
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