In the modern pharmaceutical industry, it is critically important to identify and quantify impurities with the highest possible confidence given their potential toxic effects on humans. This report describes the performance of the Agilent 6545 Q-TOF LC/MS system in the determination of metoclopramide pharmaceutical impurities. In this, the 6545 Q-TOF and 1290 Infinity LC system are used to determine metoclopramide impurities (structures below). Metoclopramide standard prepared at 500 ppm was spiked with all known impurities described in European Pharmacopoeia and two additional impurities at 0.05% (w/w) and 0.01% (w/w) levels.
【含量测定】取本品20片,精密称定,研细,精密称取适量(约相当于曲安西龙16mg),置100ml量瓶中,加甲醇适量,超声处理10min使曲安西龙溶解,放冷,用甲醇稀释至刻度,摇匀,滤过,精密量取续滤液5ml,置50ml量瓶中,用甲醇稀释至刻度,摇匀,测定。色谱条件:检测波长:UV 238 nm流动相:乙腈-水(18:82)洗脱方式:等度进样量:20 ul
通过优化保健品中L-羟脯氨酸的测定条件,建立保健品中L-羟脯氨酸的液相色谱-串联质谱(LC-MS/MS)定量检测的分析方法。方法采用酸水解的方法处理L-羟脯氨酸, 色谱柱(EC-C18,4.6 mm x 50 mm, 2.7µ m), 流动相为水相和乙腈按一定的梯度进行洗脱, 流速0.5 mL/min, 采用LC-MS/MS在正离子模式下检测, 外标法定量。高效液相色谱串联质谱法灵敏度高、 准确、 重现性好, 适用于保健品中L-羟脯氨酸的含量测定。