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Application Of Inhibitory Conductance Ion Chromatography In The Analysis Of Main/Trace Key Components Of Drugs

Posted on:2020-12-24Degree:MasterType:Thesis
Country:ChinaCandidate:K ZengFull Text:PDF
GTID:2381330605468635Subject:Polymer Chemistry and Physics
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In the field of medicine,rapid and accurate determination of main/trace key components of drugs plays an important role in drug production,quality control and functional component analysis.It is necessary to establish a specific rapid drug analysis and detection method for specific drugs.In this work,rapid and accurate methods for the determination of main/trace key components in four drugs were established by using the inhibitory conductance ion chromatograph.The specific research content is as follows:A method for the indirect determination of losartan potassium by inhibiting conductance ion chromatography was developed.This method adopts oxygen flask combustion,quartz cloth as sample coating material,glycerin as ignition agent,500 m L conical flask as container for combustion treatment.The system optimizes the parameters of the ion chromatograph to avoid the interference of other anions on chloride ion.The limit of detection?LOD,3s?of the method was 0.0852?g/m L.At the same time,the standard plant?spinach?chlorine was added to the samples,and the standard recovery was 94.47%?125.6%.The recovery of chloride ion standard solution was104.7%?116.4%,the relative standard deviation?RSD?was less than 6%.The method has high test accuracy,low background blank value and less than 30min test cycle,and can be used for rapid and accurate determination of chlorine in losartan potassium tablets.A method for the determination of Cl-,Br-and Cl2CHCOOH in polyglutamic acid grafted polyethylene glycol monoether sodium was established.Dionex Ion PacTM AS11-HC RFICTM?4*250mm?was used as the analytical column.The test conditions of Cl-and Br-in the sample were as follows:15 mmol/L sodium hydroxide solution was used as the eluent,the flow rate was 1.0m L/min,the column temperature was 30?,the inhibitory current of the suppressor was 59 m A.The test conditions of dichloroacetic acid were as follows:30 mmol/L sodium hydroxide solution was the eluent,the column temperature was 40?,the flow rate was 1.0 m L/min,the inhibitory current of the suppressor was 75 m A.The detection limits of Cl-and Br-in solution were 0.03 g/m L,the quantitative limit of Cl-and Br-in solution were 0.1 g/m L.The detection limits of Cl2CHCOOH in solution were0.3 g/m L,the quantitative limit of Cl2CHCOOH in solution were 1.0 g/m L.In addition,The recoveries of bromine ion?Br-?,chloride ion?Cl-?and dichloroacetic acid?Cl2CHCOOH?were within 100±10%,and the relative standard deviation?RSD?of the precision and repeatability were less than 5%.This method is simple in sample treatment,and the test cycle can be controlled within 20min.An ion chromatography method was developed for the determination of trifluoroacetic acid residue in laluptide with sodium hydroxide as the eluent.Dionex Ion PacTM AS11-HC RFICTM?4*250mm?was used as the analysis column,30 mmol/L sodium hydroxide solution was the eluent,the flow rate was 1.0 m L/min,the column temperature was 40 ?,and 75 m A inhibited current conductance test was performed.The detection limit of CF3COOH of this method is 3.0 g/g,the quantitative limit is 10.0 g/g.The standard recovery of spiked test is within the range of 100±10%.The sample treatment is parallel,and the relative standard deviation?RSD?are less than 5%for six analysis.This method is suitable for rapid and accurate detection of trifluoroacetic acid in laluptide with a test cycle of less than 20 min.A method for the determination of dichlorosulfoxide in p-benzoyl chloride was established based on icp-oes.The method adopts organic/water extraction in situ oxidation.The conditions for the extraction procedure were studied,and it was found that when the aqueous phase solution contained10%?V/V?nitric acid and 2%?V/V?hydrogen peroxide and the shaking time was kept in about 2 min,the full hydrolization of thionyl chloride and the complete oxidation of H2SO3 could be accomplished,as well as a quick separation of the two organic/water phase was realized.The results showed that the limit of detection?LOD,3s?of the method was 0.219 mg/kg?calculated as S?,the relative standard deviation?RSD?was 2.1%for six real sample analysis,and the recoveries of spiked test were 92.67%-104.6%.The results showed that this method met the requirements of analysis quality,and the process was simple.
Keywords/Search Tags:Ion chromatography, Conductance detection, Trifluoroacetic acid, Laluptide, Potassium losartan, Dichlorosulfoxide
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