课件：药品质量控制中的现代分析方法与技术.ppt

曲马多LC-MS/MS质谱扫描图（m/z=58） 曲马多质谱裂解图 m/z 264 ?m/z 58 单次给药 受试者单次口服苯甲酸利扎曲普坦片后，苯甲酸利扎曲普坦的Cmax和AUC与服药剂量成正比关系。 Cmax－Dose AUC－Dose 数据分析 受试者单剂量口服低中高剂量后的平均血药浓度-时间曲线 受试者单剂量口服低中高剂量后的 平均累积排泄量-时间曲线 受试者多次服药第3～6天时平均谷时血药浓度-时间曲线 受试者多次口服达稳态后的平均药时曲线 2.4 其他质谱技术与特点 创新 意识 不断 探索 勇于 实践 THANK YOU SUCCESS * * 可编辑 * This is the full-scan MS of buspirone, which yield ions characteristic of its molecular weight. * SIM passes ions of one m/z essentially 100% of the time. Hence, SIM has a high duty cycle and therefore high sensitivity relative to a lower duty cycle scan mode (e.g., full-scan MS). * Product ion scan mode is used to identify fragment ions indicative of the analyte. As a scanning technique (Q3 is scanned), this mode of operation has a low duty cycle (decreased sensitivity). * Here is the product ion spectrum of buspirone highlighting some of the structures of the fragment ions. Scan modes below will focus on the m/z 122 fragment ion of buspirone * Precursor ion scanning is the “mirror” image of product ion scan mode, whereby Q1 is scanned instead of Q3. This technique is useful in identifying different compounds that fragment to give one specific fragment ion (selected with Q3). A good example of this case is for drug metabolites. Again, since this is a scanning technique, the duty cycle is low (decreased sensitivity). * Since buspirone fragments to generate a strong m/z 122 ion (see “Product Ion Spectrum of Buspirone” slide above), an LC/MS/MS method using precursor ion scanning was employed to identify buspirone metabolites that also fragment to give a m/z 122 ion. From the chromatogram above, the precursor ion spectrum at 11.62 minutes yields an ion at m/z 402. This means that a compound with a molecular weight of 401 was ionized to give an (M+H)+ at m/z 402, which was selected with Q1, fragmented in Q2 and passed through Q3, which was fixed at m/z 122. When compared to buspirone, which eluted at 15.45 minutes, the mass difference is 16 dalton