论文部分内容阅读
目的:检查并推证表阿霉素中的有关物质。方法:采用 LC/ESI/MS联用技术测定,在Agilent 1100 LC/MSD系统上完成,其中液相色谱条件为:柱ZorbaxSB4.6mm×75mm,3μm,柱温:35℃,流动相:A）0.5％乙酸;B）甲醇-乙腈（1:1）,含0.1％乙酸,线性梯度:0～25min,25％B～45％B。流速:1mL·min-1,柱后分流:1:1,检测:UV234nm。质谱条件:离子化方式ESI（+）,扫描范围200～1200m/z,干燥气流速10L·min-1,温度350℃,雾化气压2.07×105Pa,毛细管电压 4 000 V,碎裂器电压 70 V、150 V。结果:从表阿霉素中分离出多个有关物质,其中 4个有关物质经质谱解析推导分别为表阿霉素二聚体、柔红霉素以及2个表阿霉素的同系物。结论:表阿霉素在生产过程中可生成多种结构类似物或聚合物,LC/ESI/MS作为一种高效分离与灵敏检测相结合的现代分析方法,为快速有效地检查和鉴定药品生产过程中可能产生的有关物质提供了有力的技术保证。
Purpose: To check and promote the related substances in epirubicin. Method: The LC / ESI / MS assay was performed on an Agilent 1100 LC / MSD system. The HPLC conditions were: column Zorbax SB 4.6 mm × 75 mm, 3 μm, column temperature 35 ℃, mobile phase A) 0.5% acetic acid; B) methanol-acetonitrile (1: 1) with 0.1% acetic acid, linear gradient: 0-25 min, 25% B- 45% Flow rate: 1 mL · min-1, post-column shunt: 1: 1, detection: UV234nm. Mass spectrometry conditions: ionization mode ESI (+), scanning range 200 ~ 1200m / z, drying gas flow rate 10L · min-1, temperature 350 ℃, atomization pressure 2.07 × 105Pa, capillary voltage 4 000 V, V, 150 V. Results: A number of related substances were isolated from epirubicin. Four related substances were identified as epirubicin dimer, daunorubicin and two epirubicin homologues by mass spectrometry. Conclusion: Epirubicin can generate many kinds of structural analogues or polymers in the production process. LC / ESI / MS is a modern analytical method combining high-efficiency separation with sensitive detection. In order to quickly and effectively check and identify the production of drugs The process of possible related substances provided a powerful technical assurance.