RP-HPLC法测定重酒石酸氢可酮原料药中有关物质的含量
Determination of the Related Substances in Hydrocodone Bitartrate Raw Material by RP-HPLC
李诗草 1李宏名 1杨红 1马玉洁 1蒲刚1
作者信息
- 1. 中国医药集团四川抗菌素工业研究所,成都610051
- 折叠
摘要
目的:建立测定重酒石酸氢可酮原料药中8种有关物质吗啡、双氢可待因、可待因、羟考酮、可待因酮、甲基可待因、二苯甲酮和蒂巴因的方法.方法:采用梯度洗脱的反相高效液相色谱法.色谱柱为Inertsil ODS-2,以辛烷磺酸钠-乙腈组成流动相体系进行梯度洗脱,流速为1.5 mL·min-1,检测波长为283nm,柱温为40℃.检测3批样品中的有关物质.结果:重酒石酸氢可酮与各有关物质分离良好,其中重酒石酸氢可酮、蒂巴因、二苯甲酮检测浓度线性范围分别为1.020 5～20.410 0、0.508 5～20.340、0.10～40.00μg·mL-1(r分别为0.999 7、0.999 9、1.000 0)；检测限分别为0.05、0.005、0.005 μg.3批样品中均未检出已知杂质峰.结论:本法简便、专属、灵敏,可用于重酒石酸氢可酮原料药有关物质的测定.
Abstract
OBJECTIVE: To establish a method for the determination of related substances in hydrocodone bitartrate raw material, i.e. morphia, dihydrocodeine, codeine, oxycodone. codeinone, methylcodeine, benzophenone and thebaine. METHODS: RP-HPLC method was adopted with gradient elution. The determination was Inertsil ODS-2 column with mobile phase consisted of sodium octanesulphonate-acetonitrile (gradient elution) at the flow rate of 1.5 mL·min‐1. The detection wavelength was set at 283 on, and column temperature was 40 ℃.. Related substances in 3 batches of samples were determined. RESULTS: Hydrocodone bitartrate was completely separated from related substances. The calibration curve of hydrocodone bitartrate was linear within 1.020 5~ 20.410 0 μg·mL‐1 (r=0.999 7). The linear ranges were 0.508 5~20.340 μg·mL‐1 for thebaine (r=0.999 9) and 0.10~40.00 μg· mL‐1 for benzophenone (r= 1.000 0). The limits of detection were 0.05 μg for hydrocodone bitartrate and 0.005 μg for thebaine and benzophenone. Known impurity peak hadn't been detected in 3 batches of samples. CONCLUSION: The method is simple, selective and sensitive for the determination of related substances in hydrocodone bitartrate raw material.
关键词
反相高效液相色谱法/重酒石酸氢可酮/有关物质/梯度洗脱Key words
RP-HPLC/Hydrocodone bitartrate/Related substances/Gradient elution引用本文复制引用
出版年
2012
国家科技期刊平台
NSTL
维普
万方数据