摘要
目的建立顶空气相色谱法测定异维A酸原料药中10种残留溶剂的方法。方法采用程序升温法,色谱柱为DB-624毛细管柱(30 m×0. 32 mm,1. 8μm),进样口温度200℃,氢火焰离子化检测器温度250℃,载气为氮气,流速2. 0 mL·min-1,分流比5∶1,顶空平衡温度90℃,平衡时间30 min,进样体积1. 0 m L。结果 10种有机溶剂的分离较好,浓度在试验范围内与峰面积具良好的线性关系,r为0. 9994～0. 9999,回收率均在80%～120%,RSD均<10%,检测限为0. 098～4. 17μg·mL^(-1),定量限为0. 33～13. 91μg·mL^(-1)。结论所用气相色谱法适用于异维A酸原料药中残留溶剂测定。
OBJECTIVE To establish a headspace GC method for the determination of residual organic solvents in Isotretinoin.METHODS The residual solvents were separated on DB -624 capillary column (30 m × 0.32 mm,1.8 μm)by programmed temperature.The inlet temperature was 200℃ and the FID temperature was 250 ℃.Nitrogen was used as carrier gas with flow rate of 2.0 mL·min^-1 and the split ratio was 5 :1.Headspace oven was kept heating at 90℃ for 30 min.The injection volumn was 1.0 mL.RESULTS 10 solvents could be separated in the chromatogram and the calibration curve of each solvent was linear within certain range.The recoveries were within 80%-120% with the RSDs less than 10%.LODs were within 0.098 -4.17 μg·mL^-1 and LOQs were within 0.33 -13.91 μg·mL^-1.CONCLUSION The method can be applied to the determination of residual solvents in Isotretinoin.
作者
唐杨
TANG Yang(Chongqing Engineering Research Center for Pharmaceutical Process and Quality Control,Chongqing Institute for Food and Drug Control,Chongqing ,401121 P.R.China)
出处
《华西药学杂志》
CAS
CSCD
2019年第1期58-62,共5页
West China Journal of Pharmaceutical Sciences
基金
国家药典委员会国家药品标准提高研究项目(编号:[2016]141)
关键词
异维A酸
原料药
顶空
气相色谱
程序升温
残留溶剂
含量
测定
Isotretinoin
API
Headspace
GC
Programming temperature
Residual solvents
Content
Determination
