【正文】 Sheath gas pressure: 45 Auxiliary gas pressure: 15 Ion transfer capillary temperature: 300 oC Source CID: 8 V Scan Type: SRM, 3 transitions of [MH](m/z: 321) (321?152, 321 ? 194 and 321 ? 257) Q1 peak width Da in SRM or Da in HSRM Q3 peak width Da Collision Pressure: Ar at mTorr O HO HN HHHOClClO2NQ1 peak width and HSRM experiment Enabling the HSRM experiment Highly Selective Selected Reaction Monitoring (HSRM) Reduces ―isobaric‖ chemical noise Increases confidence of analysis amp。 Chlroamphenicol(氯霉素， CAP)殘留測(cè)定 HPLC analysis was performed on the Finnigan Surveyor HPLC module with MS Pump and Autosampler –Column: Thermo Hypersil Gold C18 (100 mm, 5181。此外，尚可外用治療痤瘡、酒糟鼻、脂溢性皮炎等。 its application in pharmaceutical analysis GCFTIR GCMS UPLCMS HPLCNMR Hyphenated Techniques in Chromatography 現(xiàn)代聯(lián)用技術(shù)及其應(yīng)用 HPLCMS CEMS + + 樣品與溶劑脫 離及電離 EI ? ESI ? APCI LC/MS 接口 離子源 質(zhì)量分析器 檢測(cè)離子 HPLC 數(shù)據(jù)系統(tǒng) 質(zhì)譜 離子識(shí)別 ? Quadrapole ? Time of Flight ? Fourier Transform ? … + + + + + + + 離子檢測(cè) + + + + + + + + + + + 第二節(jié) 液質(zhì)聯(lián)用技術(shù)與應(yīng)用 離子化方式 離子分離與測(cè)定模式 FullScan Mass Spectrometry ? Advantage – Provides MW Information FullScan MS of Buspirone NNNNNOOBuspirone (丁螺環(huán)酮 ) C21H31N5O2 MW = 385 150 200 250 300 350 400 450 500 m/z 25 50 75 100 Relative Abundance 386 408 (M+H)+ (M+Na)+ Single Ion Monitoring (SIM) ? Advantages – Targeted Analyte Monitoring – High Duty Cycle – Simple ? Disadvantages – Can suffer from interferences – Not as sensitive or selective as SRM (see below) Fixed m/z Pass All Pass All Product Ion Scanning: A Tandem MS Method ? Advantage – Provides Structural Information ? Disadvantage – Low duty cycle Fixed m/z Pass All Scanning Product Ion Spectrum Q3 Q2 Q1 Product Ion Spectrum of Buspirone NHNNNOON HNOO100 150 200 250 300 350 400 m/z 25 50 75 100 Relative Abundance 122 386 222 150 265 180 NNNNHNOO(M+H)+ Precursor Ion Scanning ? Advantage – ID pounds producing specific fragment ion (., PO3? for phosphopeptides) ? Disadvantage – Low duty cycle Fixed m/z Pass All Scanning Precursor Ion Spectrum Q3 Q2 Q1 Precursor Ion Scan Mode for Buspirone Metabolites Precursor Ion Scan: Q3 set to m/z 122 N NNNNOOOH100 200 300 400 500 m/z Relative Abundance 402 386 9 10 11 12 13 14 15 16 Time (min) 25 50 75 100 Relative Abundance N NNNNOONHNNNeutral Loss Scanning ? Advantage – Screen for pounds producing specific neutral loss (., loss of 176 for glucuronide conjugates) ? Disadvantage – Low duty cycle Scanning Pass All Scanning Neutral Loss Spectrum Linked Q3 Q2 Q1 Neutral Loss Scan of Buspirone Metabolites Neutral Loss Scan: Q1/Q3 difference set to 121 Da 100 200 300 400 500 m/z Relative Abundance 402 386 9 10 11 12 13 14 15 16 Time (min) 25 50 75 100 Relative Abundance N NNNNOON NNNNOOOHSelected Reaction Monitoring (SRM) ? Advantages – Targeted Analyte Monitoring – High Duty Cycle – “Simultaneous” Monitoring of Multiple Transitions ? Disadvantage – No “advanced” structural information Fixed m/z Pass All Fixed m/z Q1 Q2 Q3 MS/MS Selectivity in Complex Matrices 息斯敏 ——阿斯咪唑 (astemizole) ? Chlroamphenicol(氯霉素， CAP)殘留測(cè)定 ? 黃楊生物堿成分鑒定 ? 苯甲酸利扎曲普坦人體藥代動(dòng)力學(xué)研究 O HO HN HHHOClClO2NC11H12Cl2N2O5 FMW= 【 類別 】 酰胺醇類抗生素 【 適應(yīng)癥 】 本品是治療傷寒、副傷寒的首選藥物，外用可治療沙眼。 ) technology starts with unique 181。 its application 藥物現(xiàn)代色譜法及其應(yīng)用 UPLC UltraPerformance LC174。 現(xiàn)代光譜技術(shù)： 藥物結(jié)構(gòu)鑒定， 微量雜質(zhì)檢定。 色譜及其聯(lián)用技術(shù)： 藥學(xué)研究－－分子水平。藥品質(zhì)量控制中的 現(xiàn)代分析方法與技術(shù) Modern analytical methods amp。 techniques in quality control of drugs 第十六章 現(xiàn)代分析方法與技術(shù)，為藥學(xué)的發(fā)展提供了適時(shí)而有效的手段與動(dòng)力。 手性分析： 毛細(xì)管電泳及手性色譜技術(shù)－－藥物研究與質(zhì)量控制提供了保障。 第一節(jié) 概況 Capillary electrophoresis,CE Modern chromatogr amp。 (UPLC174。m smallparticle chemistries. Chromatographers no longer need to choose between speed and resolution—with UPLC you get both. Mass spectroscopy MS Nuclear magic resonance spectrometry NMR Xray diffraction method Near infrared spectrometry NIRS 現(xiàn)代光譜法及其應(yīng)用 Modern spectroscopy amp。因腦脊液濃度高，故常用于治療細(xì)菌性腦膜炎和腦膿腫。 被農(nóng)業(yè)養(yǎng)殖濫用！ 肉食品中嚴(yán)格檢查。) –Mobile Phase: A: Water。 improved LOQ Q1 peak width Da in SRM or Da in HSRM Q3 peak width Da O HO HNHHOClClO2NO NHHNOClClO HON HHHOClClO2NO HO2NOHCO2NO HHm / z 3 2 1m / z 2 5 7m / z 3 2 1m / z 1 9 4m / z 1 5 2CAP SRM Result: CAP Standard Q1 peak width = Da R T : 0 . 0 0 5 . 0 00 . 0 0 . 2 0 . 4 0 . 6 0 . 8 1 . 0 1 . 2 1 . 4 1 . 6 1 . 8 2 . 0 2 . 2 2 . 4 2 . 6 2 . 8 3