Study On The Gel Preparation Quality Control And Characterization Of The Key Technology

The gel preparation is a new drug dosage emerging in recent years, because of its good biocompatibility, good absorption, good stability, no pollution to the clothes with the local administration; the characteristics of drug release is controlled release, sustained release effect and is widely applied. In order to ensure the safety and effectiveness of drugs, the study of quality control is the key. The existence of high polymer used in the process of preparation of pharmaceutical excipients not only interferes with the measurement of small molecules active substances, but also increases the difficulty of its quality characterization. Therefore, in the sample pretreatment of gel content, characterization of small molecule active substance is an urgent problem and attractes the attention of many researchers try to do some more.At present, gel preparation sample pretreatment methods including gel osmosis, organic solvent extraction and centrifugal settling. However these methods are time consuming and tedious operation process, and the separation effect is not ideal, the accuracy and reliability of analysis is not high. Ultrafiltration is a mean of sample treatment and it is usually used at present, which is mainly under the influence of pressure, retaining macromolecular, make small molecules to pass through the ultrafiltration membrane, so as to realize the separation of macromolecules and small molecules. By using ultrafiltration traditional are flat membrane filtration, the centrifugal ultrafiltration process is easy to produce the phenomenon of concentration polarization and membrane, lead to reduce seepage flow and separation efficiency, influence the accuracy of the analysis. Hollow fiber ultrafiltration(HFCF-UF) is a new type of ultrafiltration technology, which overcomes the phenomenon of concentration polarization conventional ultrafiltration method, greatly improving the separation efficiency. The separation of HFCF-UF has been successfully applied in pharmaceutical formulations and biological fluids of small molecular active substances, showing the separation of small molecules in the foreground in complex matrices. However the complex mechanism of the application has not been reported in gel.In order to ensure the accurate quantification of effective components in compound gel, to research and develop a simple, suitable for the routine quality control of the pretreatment method is an important topic for researchers, and also a key problem to ensure the future development and application of gel preparation.This subject, represented by ketoprofen gel and ofloxacin gel, through the study of hollow fiber on the drug adsorption and gel preparation diluent selection, did the research on gel preparation quality control and characterization of the key technology. The research results show that HFCF-UF pretreatment method for the analysis of gel preparation of small molecular substances, has the advantages of high efficiency, simple and fast, which can be used to overcome the shortcomings of traditional methods, such as fussy operation and the separation effect not ideal. It provides a reliable analysis platform for the characterization of small molecules in gel preparation containing polymer materials.Part 1 Content determination of the principal agent Ketoprofen Gelmethod in the first part- high performance liquidchromatography of hollow fiber ultrafiltrationObjective: to establish a hollow fiber ultrafiltration(HFCF-UF), on the content of main drugs in Ketoprofen Gel analysis.Methods: first, using HFCF-UF multi sample purified by separation, separation and purification conditions of HFCF-UF device: centrifugation at 4000 r/min 15 min, remove the hollow fiber, collecting cavity solution, direct HPLC analysis. Chromatographic conditions: phenomenexc C18column(250 x 4.60 mm); mobile phase: 0.05 mol- L-1 potassium dihydrogen phosphate(value to 3.5 with phosphoric acid to regulate p H)- methanol(25:75); flow rate: 1 m L- min-1; column temperature was room temperature; the detection wavelength: 255 nm; sample size: 20 L.Results: good chromatographic system adaptability and exclusive; ketoprofen in 0.26 ~ 10.2 G- m L-1 linear relation in the range of good; precision and repeatability test: RSD is less than 0.2%, show that the method is good precision; ketoprofen average recovery rates were: 101.1%(RSD=1.3%), 102.6%(RSD=1.5%), 100.8%(RSD=1.6%); external standard method for the calculation of ketoprofen content in the sample were sample 100.5% of labeled amount, 99.8%, 99.7%.Conclusion: this method has the advantages of high efficiency, convenient, fast, to overcome the traditional method of fussy operation, the separation effect is not ideal shortcomings, provides a reliable analysis platform for the characterization of small molecules in gel preparation containing polymer materials. Part 2 Content determination of the principal agent Ofloxacin Gelmethod in the second part- high performance liquidchromatography of hollow fiber ultrafiltrationObjective: to establish a hollow fiber ultrafiltration(HFCF-UF), on the content of main drugs in Ofloxacin Gel analysis.Methods: first, using HFCF-UF multi sample purified by separation, separation and purification conditions of HFCF-UF device: centrifugation at 4000 r/min 15 min, remove the hollow fiber, collecting cavity solution, direct HPLC analysis. Chromatographic conditions: Promosil C18 column(150 x 4.60 mm); a mobile phase of methanol: water(30:70, three triethylamine, containing 0.5% adjusted to p H 4 with phosphoric acid); flow rate: 1 m L- min-1; column temperature was room temperature; the detection wavelength: 293 nm; sample size: 20 L.Results: good chromatographic system adaptability and exclusive; ofloxacin in 5.10 ~ 51 G- m L-1 linear relation in the range of good; precision and repeatability test: RSD is less than 0.5%, show that the method is good precision; the average recovery rate of ofloxacin were 101.1%(RSD=1.7%), 99.9%(RSD=0.8%), 100.3%(RSD=0.9%); external standard method to calculate the content of ofloxacin samples as the sample of the labeled amount of 101.5%, 100.4%, 99.6%.Conclusion: with efficient, convenient, fast, to overcome the traditional method of fussy operation, the separation effect is not ideal shortcomings, provides a reliable analysis platform for the characterization of small molecules in gel preparation containing polymer materials.