16第十六章药品质量控制中的现代分析方法与技术.pptx

药品质量控制中的现代分析方法与技术;;Capillary electrophoresis,CE;UPLC;Mass spectroscopy MSNuclear magnetic resonance spectrometry NMRX-ray diffraction methodNear infrared spectrometry NIRS;GC-FTIR;;2.1 离子化方式;;;;;2.2 离子分离与测定模式;;Full-Scan Mass Spectrometry;Full-Scan MS of Buspirone;Single Ion Monitoring (SIM);Product Ion Scanning: A Tandem MS Method;Product Ion Spectrum of Buspirone;Precursor Ion Scanning;Precursor Ion Scan Mode for Buspirone Metabolites;Neutral Loss Scanning;Neutral Loss Scan of Buspirone Metabolites;Selected Reaction Monitoring (SRM);MS/MS Selectivity in Complex Matrices;Chlroamphenicol(氯霉素，CAP)残留测定 黄杨生物碱成分鉴定 苯甲酸利扎曲普坦人体药代动力学研究;C11H12Cl2N2O5 FMW=323.13;HPLC analysis was performed on the Finnigan Surveyor HPLC module with MS Pump and Autosampler Column: Thermo Hypersil Gold C18 (100×2.1 mm, 5μ) Mobile Phase: A: Water; B: Acetonitrile Column Temperature: 40 oC Gradient Program: 0.25 mL/min Injection: 20 uL with loop;Operation Conditions for CAP;Q1 peak width and H-SRM experiment;;CAP SRM Result: CAP Standard Q1 peak width = 0.7 Da;CAP SRM Result: Kidney Blank ;CAP SRM Result: Kidney Spiked (0.5ng/g);CAP H-SRM Result: CAP Standard Q1 peak width = 0.2 Da;CAP H-SRM Result: Kidney Blank;CAP H-SRM Result: Kidney Spiked (0.5ng/g);2.3.2 黄杨宁生物碱HPLC-MS联用鉴定;黄杨生物碱HPLC-ELSD色谱图 ;环维黄杨星D和有关生物碱含量测定结果;环维黄杨星D及其有关生物碱的鉴别 质谱条件 电喷雾离子化正离子检测 喷口电压5000V 雾化气压35psi 辅助气压力5psi 毛细管温度350℃ 碰撞气氩气压力1.5mTorr 色谱条件 色谱柱：Lichrospher SiO2 (250mm×4.6mm,5 μm) 流动相：四氢呋喃-甲醇-乙腈-氨水 ( 32:50:13:3) 流速：1mL·min -1 柱温：30℃;黄杨宁LC-MS/MS全扫描色谱图 ;峰1母离子质荷比;可能为峰1的黄杨宁有关生物碱;峰2母离子质荷比;可能为峰2的黄杨宁有关生物碱;峰3母离子质荷比;可能为峰3的黄杨宁有关生物碱;峰4母离子质荷比;峰5母离子质荷比;可能为峰5的黄杨宁有关生物碱;峰6母离子质荷比;峰7母???子质荷比;峰8母离子质荷比; 357.15;m/z=375;;峰9二级质谱图;m/z=389;峰位号 ;苯甲酸利扎曲普坦 (Rizatriptan Benzoate) MW: 391.47 分子式：C15H19O5·C7H6O2;药理作用;实验内容;LC-MS/MS测定方法建立;色谱条件;空