摘要
目的建立注射用米卡芬净钠中残留溶剂丙酮的测定方法。方法采用顶空毛细管气相色谱法，DB-624石英毛细管柱，检测器为氢火焰离子化检测器，载气为氦气，流速为3．0mL／min，柱温采用程序升温（起始温度50℃，维持8min，再以40℃／min的速率升温至210℃，维持6min），进样口温度为140℃，检测器温度为260℃，顶空温度为80℃，平衡时间为30min，分流比为2：1，定量环温度为100℃，传输管温度为110℃，进样体积为1mL。结果残留溶剂丙酮在该色谱条件下专属性高，在13．331-142．20μg／mL的范围内，丙酮的峰面积与浓度呈现良好线性关系（r=0．9998），平均回收率为101．1％（RSD=1．7％），检测限为0．26662gg／mL，定量限为0．53325μg／mL。结论该方法简便、准确、可靠、灵敏，可用于注射用米卡芬净钠中残留溶剂丙酮含量的测定。
Objective To establish a method for the determination of residual solvent acetone in micafungin sodium for injection. Methods Headspace capillary GC method was adopted. The determination was performed on a DB-624 capillary column at the rate of 3.0mL/min using helium gas as carrier gas and FID as the detector by temperature programming（initial column temperature of 50℃, maintaining for 8min, then raising to 210℃ at a rate of 40℃/vain, maintaining for 6min）. The temperature of the injector was maintaining at 140℃ and that of detector at 260℃. The equilibrium temperature was 80℃ and equilibrium time was 30min. The split ratio was 2：1. The looper temperature was 100℃ and the transmission pipe temperature was 110℃. The volume of sample was lmL. Results The residual solvent acetone exhibits a high specificity. The calibration curve showed a good linear relationship with the linear range of 13.331-142.20μg/mL（r=0.9998）. Average recovery was 101.1%（RSD= 1.7%）, the LOD and LOQ were 0.26662 and 0.53325gg/mL, respectively. Conclusion The method is simple, accurate, reliable and sensitive, and suitable for the determination of residual solvents in micafungin sodium for injection.
出处
《中国抗生素杂志》
CAS
CSCD
北大核心
2016年第5期352-355,共4页
Chinese Journal of Antibiotics
关键词
顶空毛细管气相色谱法
注射用米卡芬净钠
残留溶剂
丙酮
Micafungin sodium for injection
Residual solvent
Headspace capillary gas chromatography
Acetone
