hplc最终方法.doc

ComparisonbetweenthetwoValidatedHPLCmethodsforPMIDApuritydetermination两种已验证的测定双甘膦纯度的HPLC方法的比较ForthepuritydeterminationofPMIDAbyHPLCtechnique,twoseparatedmethodsweredevelopedandvalidatedfollowingprocedureweredefinedinagreementwithICH(InternationalConferenceonHarmonization)rules“ValidationofAnalyticalMethod:DefinitionandTerminology”针对HPLC技术测定双甘膦的纯度,研发并验证了两种不同的方法,按照ICH(国际协调会)条例“分析方法的验证:定义和术语”来确定以下步骤。Thetwomethods,respectivelyreportedinReport048/11and140/11,(流动相)。Inboththemethods,,分析时间是可对比的并且从验证中获得的参数非常有可比性。Asummaryofanalyticaldatacollectedforeachofthemarefollowingreported:收集的两种方法的分析数据汇总报告如下:Report048/11withStrongIonExchangecolumn报告048/11,onditions色谱条件Instrument: HPLCAgilent1100仪器:HPLC安捷伦1100Column: µm柱:µmMobilephase: 85%(250mMKH2PO4pH2)÷15%(MeOH)mixed流动相:85%(250mM磷酸二氢钾pH2):15%(甲醇)的混合物Flow: :: 20mL注入体积:20mLColumntemperature: 25°C柱温:25°CDetector: UV-visibleat195nm探测器:195纳米的可视紫外线Analysistime: :(85%(250mMKH2PO4pH2)÷15%(MeOH)mixed)85%(250mM磷酸二氢钾pH2):15%(甲醇)的混合物Referencesoltution(S)参比溶液(S)20mgofPMIDAstandard,accuratelyweighted,。SampleSolution(C)样品溶液(C)20mgonthesample,accuratelyweighted,。Sequenceofinjections注入顺序Thesolutionshavetobeinjectedintheinstrumentinthefollowingsequence:溶液必须按照以下顺序注入到仪器中:Blank 3injection空白溶液3次注入ReferenceSolution(S) 2injection参比溶液(S)2次注入Blank 1injection空白溶液1次注入SamplePreparation(C) 2injection样品溶液(C)2次注入Retentiontime保留时间ChromatogramofPMIDAsolution(=)双甘膦溶液(双甘膦浓度=),,(min)保留时间(分钟)