有关物质分析中hptlc与hplc的相关性研究-药物分析专业论文.docx

压为120V,m/z扫描范围为100～500。4、利用MassWorks软件建立HPTLC-MS与HPLC-MS质谱数据的相关性利用MassWorks软件分别对加替沙星及其8种有关物质在HPTLC-MS 和HPLC-MS 分析中获得的准分子离子峰进行校正，计算校正后同位素峰形曲线的相似度，得出不同方法中同一物质的最小相似度值，作为HPTLC与HPLC相关性分析的阈值（97%），以实现在HPLC与HPTLC系统中对元素组成相同的物质的相互相关。二、通过对洛美沙星和环丙沙星降解产物的分析，进一步验证HPTLC 与HPLC 相关性分析方法分别建立了分析洛美沙星和环丙沙星诸降解混合溶液的HPTLC-MS和HPLC-MS方法，按上述方法将各杂质的准分子离子峰进行MassWorks校正后，计算峰形校正曲线的相似度，洛美沙星的10个降解杂质在HPTLC和HPLC色谱图中可以逐一得到对应；环丙沙星在HPTLC-MS和HPLC-MS分析中可检测到的3个有关物质在两种色谱系统中也得到了逐一对应。本论文的工作说明，利用HPTLC-MS和HPLC-MS技术，通过MassWorks软件，可以方便地实现HPTLC与HPLC色谱图中诸色谱峰的逐一对应，为利用HPTLC作为互补方法，验证RP-HPLC方法的分离能力提供了解决方案。关键词：HPTLC，HPLC，有关物质，相关AbstractRP-HPLCisoneofthemostimportantmethodinthecontrolofdrugrelatedsubstance.Theseparation abilityofchromatographicsystemshouldbeverifiedinestablishingtheRP-HPLCmethod.Theeffectiveness oftheHPLCmethodcanbeevaluatedbythecorrelationwithotheranalyticalmethodsofdifferentprinciples,suchasNP-HPLC、HPTLC、HPCE.ThispaperistostudythevalidationmethodfortheseparationabilityofRP-HPLCsystemwithHPTLCasacomplementarymethod,bymeansofthecorrelationresearchbetween HPTLCandRP-HPLCinanalysisofquinoloneantibioticsrelatedsubstance.Thecontentissumarizedas follows:1、EstablishmentofthecorrelationresearchmethodbetweenHPLCandHPTLCwithgatifloxacinanditsrelatedsubstanceas examplesTheestablishmentofHPTLCseparationmethodforgatifloxacinandits9relatedsubstance.Basedontheexperimentaldesign,theHPTLCmethodwasestablishedandoptimized.Thepreliminary screeningdevelopingsystemwascarriedoutbyahomogeneousdesignfromthe22kindsofcommonTLC solvents.The percentage of the developing system was optimized by a central composite design. Theoptimalizingdevelopingsolvent was methanol：1，2-dichloroethane：ammonia water(15%)：acetonitrile(V/V/V/V)=2.8：7.2：0.5：0.5.TheHPTLCmethodwasasfollows:thesolidphaseistheMERKHPTLCplate（10×10cm）prewashedbymethanolandactivatiedat110。C for1h. Thespotwas 3mmwith10μLsample.It wasdevelopedatroomtemperature.Thewavelengthwas292nminthemodeofUVdetection.HPTLC-MSmethodfortheanalysisofgatifloxacinrelatedsubstance.HPTLC-MSmethod wa