藿香正气软胶囊中槟榔碱的限量检查方法研究

Study on limit test method of arecoline in huoxiang zhengqi ruanjiaonang

目的:建立藿香正气软胶囊中槟榔碱的限量测定方法。方法:采用GC-MS结合选择离子检测模式(SIM)定性,外标定量。色谱柱为DB-1MS柱(30 m×0.25 mm,0.25μm),载气为氦气;进样口温度290℃;程序升温;分流进样,分流比10∶1。传输线温度280℃;离子源温度200℃;EI源,70 e V;定性离子96、140、42、53、155、81,定量离子96;溶剂延迟2.85 min。结果:槟榔碱在0.517 5~31.05μg/ml的范围内呈良好的线性关系(r=0.999 8),平均回收率96.15%,RSD为0.5%,检出限0.1μg/ml,定量限0.3μg/ml,精密度、稳定性良好。结论:该方法稳定可靠,可作为藿香正气软胶囊中槟榔碱的质量控制方法。

Objective: To establish a test for determining the limit of arecoline in Huoxiang Zhengqi Ruanjiaonang. Methods:GC-MS combined with selective ion detection mode( SIM) was used. A GC-MS method was developed with DB-1 MS capillary column( 30 m × 0. 25 mm,0. 25 μm) as stationary phase and helium as carrier gas. The temperature of the injector was set at290 ℃. Programmed temperature upgrade was used,and the split ratio was 10∶ 1. The temperature of the transmission and ion source were set at 280 ℃ and 200 ℃,respectively. The ion source was EI and the energy was 70 ev. Qualitative ions were 96、140、42、53、155、81 and quantitative was 96. Solvent cut time was 2. 85 min. Results: The calibration curves showed a good linear relationship within the range of 0. 5175-31. 05 μg/ml of arecoline. Average recovery was 96. 15%. The limit of detection and limit of quantification were 0. 1 μg/ml and 0. 3 μg/ml,respectively. Precision and stability was good. Conclusion: The method is proved to be stable and reliable. It can be used for quality control of arecoline in Huoxiang Zhengqi Ruanjiaonang.