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High Performance Liquid Chromatography Coupled With Resonance Rayleigh Scattering For The Analysis Of The Pharmaceuticals

Posted on:2014-02-24Degree:MasterType:Thesis
Country:ChinaCandidate:J X TangFull Text:PDF
GTID:2231330398484928Subject:Analytical Chemistry
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High performance liquid chromatography (HPLC) is a kind of important separation and analysis technology, and the development of new type of detectors is also the direction of HPLC technique. In recent years, the resonance Rayleigh scattering (RRS) has been widely used in drug research as a new type of spectral analysis technology, but the RRS can not distinguish substances with similar functional groups from each other. The article will discuss HPLC coupled with RRS, which combine the advantages of high separation and high sensitivity of those technologys. It can increase the accuracy of the experiment, and realize analysis in mobile phase for RRS. Therefore, further research and development for HPLC-RRS detection has significant meanings in the application of analytical chemistry.It is undoubtable that HPLC-RRS is of great significance to promote the analysis of RRS and the development of novel HPLC detectors. This article established HPLC-RRS methods for determination of isepimicin, neomycin sulfate and torasemide. Detections of different drugs obtained good effects. This paper consists of introduction and research reports, and the research reports is divided into three parts includes2-4chapters in detail.Chapter1:IntroductionThe introduction part briefly describes the HPLC, a brief overview of RRS, improved HPLC-RRS detection device, the application of liquid chromatography coupled with derivative technology, as well as the research progress of HPLC-RRS detection and prospect of the future.Chapter2:High performance liquid chromatography (HPLC) method coupled with resonance Rayleigh scattering detection for the determination of isepamicinA simple and novel reversed-phase high performance liquid chromatography (HPLC) method coupled with resonance Rayleigh scattering (RRS) was developed to analyze isepamicin (ISP) in rat plasma. The chromatographic separation was achieved at30℃on a reverse phase column of Synergi Hydro-RP (150mm×4.6mm;4mm), with (15:85, v/v) methanol-water (containing0.15% TFA (v/v)) as the mobile phase. The flow rate was0.4mL min-1. The RRS signal was detected at λex=λem=372nm. Netilmicin (NTL) was used as the internal standard. The new analytical technique was validated for the intra-and inter-day variation, the liner range of the standard curve of ISP and the limit of detection (S/N=3). The result indicated that HPLC coupled with RRS was a reliable and valuable technique for quantitative analysis of ISP in rat plasma. The method showed a better liner relationship and lower analysis time.Chapter3:High performance liquid chromatography coupled with resonance Rayleigh scattering for determination of neomycin sulfate without organic solventA simple and rapid reversed-phase high performance liquid chromatography method, using resonance Rayleigh scattering detection, for the determination of neomycin sulfate in serum sample was developed. Neomycin sulfate could react with trypan red to form ion-association complexes, and the reaction was under non-organic solvent condition. Scanning electron microscope result that these aggregates were spherical gathered particles with an average size of45nm, which was in agreement with the theoretical results. Herein we demonstrated a novel method for determination of neomycin sulfate which obtained satisfactory results.Chapter4:High performance liquid chromatographic (HPLC) technique combinated resonance Rayleigh scattering method for determining torasemide in the serumThis method was developed to analyse the torasemide in human serum using HPLC-RSS technology. The chromatographic separation was achieved at30℃on a reverse phase column of Synergi Hydro-RP (150mm×4.6mm;4nm), with (15:85, v/v) methanol-water (containing0.2%TFA (v/v)) as the mobile phase, the flow rate was0.4mL min-1 and the scattering detection wavelength was at332nm. In weak acidic medium, CR combined with TOB to form an ion-association complex by electrostatic interaction, hydrophobicity and charge transferring effect. Within the scope of0.08to20.54μg mL-1, the determination of torasemide had good linear relationship within a certain range (r=0.9989), and the average recovery was98.9%(RSD). The experiment used this method to determine the torasemide was simple, rapid and had a good linear relationship.
Keywords/Search Tags:High performance liquid chromatography, Resonance Rayleigh scattering, Simultaneous determination, ion-association complex
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