论文部分内容阅读
缬草三酯属于多酰基类环烯醚萜化合物.中国药典2010年版一部蜘蛛香项下收载缬草三酯作为质量控制对照品使用.然而,结构不稳定是该类对照品发放中亟待解决的问题.本文通过高效液相色谱-质谱联用的方法对缬草三酯的稳定性进行了研究.根据ICH导则要求,使用加速稳定性实验对缬草三酯适宜贮存条件、运输和实验条件进行研究.结果表明,缬草三酯在碱性和加热条件下不稳定,而在酸性、氧化和强光照射条件下保持相对稳定.实验中有九个缬草三酯降解产物被检出,其中N1-N4为碱性水解时产生,B1-B5为热降解中产生.研究结果为本对照品的稳定性分析提供了依据.本文还对缬草三酯的制备、贮藏和使用等条件进行研究,该对照品在避光低温(-20％C)条件下贮藏.通过长期稳定性研究,在拟定的贮藏条件下,缬草三酯在3年内可以保持稳定.“,”Valtrate is the main drug quality control for the qualitative and quantitative analysis of Valerian medicines in the Chinese Pharmacopoeia 2010.However,valtrate is unstable under some conditions.We,for the first time,systemically evaluated the stability of two bath reference standards (RS) by high performance liquid chromatography coupled with a triple quadrupole mass spectrometer (HPLC-MS/MS).The forced degradations of valtrate were performed to evaluate its optimal storage,transportation and experiment conditions according to ICH guideline.The developed HPLC method was validated to determine the degradation products.Valtrate RS was sensitive to alkaline and thermal conditions,but it was relatively stable under acidic,oxidation and photolysis conditions.A total of nine degradation components were identified under alkaline hydrolysis (N l-N4) and thermal degradation (B1-B5).The information obtained in this work would be valuable to minimize the decomposition of valtrate during the processes of preparation,storage,distribution and utilization.It was highly suggested to store valtrate with a single dose packing in brown closed ampoule at-20 ℃C.Under the above-mentioned storage condition,valtrate could be stable for up to 3 years.