LCMS(ESI)的基本原理及应用.ppt

步骤 5－气相中的离子反应 通过离子传输区域时从大气压喷雾室的反应中会发生质子转移和电荷交换反应。这个高压区允许发生1000次离子/分子反应。  质子转移 与HPLC添加剂相比，如：氨、三乙胺（质子亲合力分别为206和232 kcal/mole ），样品具有较低质子亲合力的会丢失一个质子，变成中性或形成加合离子，如[M+NH4]+ 帽电压 裂解区 雾化气压力 干燥气 温度和流速 雾化气压力 200 ?L/min 10-20 psig 200-400 ?L/min 20-30 psig 400-800 ?L/min 30-50 psig 800 ?L/min 50-70 psig 干燥气流速 (6-12 L/Min) 含水高需更高的流速 如果太底，液滴会导致谱图中的尖峰 干燥气温度 蒸汽压越低的溶剂温度越高 开始为 300 - 350?C 帽电压 用FIA优化 (2000-5000) 开始 3000 V 在负离子模式，注意高的室电流或兰色光辉（电晕针显示）：当这现象发生时须降低帽电压 电喷雾喷雾室设置 由于液滴不完全干燥导致的尖峰 在ES中干燥气设置的作用 液滴产生噪音更大的谱图 在ES中干燥气设置的作用 含杂原子的样品 通过引入可接受一个电荷的化合物 在溶液中是多电荷的样品 在溶液中是离子的化合物 适用于热喷雾的样品 当不能引入电荷时避免极其非极性的样品 适合电喷雾的样品 * ) * * Over the past several decades, a number of different LC/MS interfacing techniques have been developed in an effort to address the requirements of an ideal LC/MS interface. The two relatively recently developed and closely related Atmospheric Pressure Ionization (API) techniques of APCI and API-Electrospray together encompass by far the broadest range of analyte polarity and molecular weight. These techniques also provide superior sensitivity and robustness compared to older techniques such as thermospray, particle beam, and FAB. For these reasons, APCI and Electrospray have rapidly become the predominant LC/MS interfaces. It is important to note that many analytes will work by either interface! * The steps need to be clearly labeled so that the student understands the order in which they happen. These slides need to be approached from the point that these settings are for the Agilent Trap which has different ionization characteristics than that of a LCQ Deca. The users we get will be LCQ users that have lots of experience with LCQs and possible experience with the Quad MSD system. For Instructor Notes * * Column: Supelcosil ABZ+Plus 5 μm, 2.1 mm x 250 mm (Supelco) Column temperature: 40 °C Mobile phase: isocratic at 25% A in B A: Acetonitrile (MeCN)  B: 5 mM TDFHA in waterFlow: 0.2 ml/min Inje