摘要
目的：建立同时测定尼莫地平缓释片中乙醇和丙酮残留量的方法。方法：采用顶空气相色谱法。色谱柱为以6%氰丙基苯基-94%二甲基聚硅氧烷（DB-624）为固定液的毛细管柱,程序升温,进样口温度为230℃,检测器为氢火焰离子化检测器,检测器温度为250℃,载气为氮气,流速为2.0 ml/min,分流比为5∶1,顶空加热温度为90℃,平衡时间为20 min,顶空进样量为1.0 ml。结果：乙醇、丙酮检测质量浓度线性范围分别为1.25-500.0μg/ml（r=0.999 9）、0.50-202.0μg/ml（r=0.999 2）;定量限分别为5.01、2.02μg/ml,检测限分别为1.67、0.67μg/ml;精密度、稳定性、重复性试验的RSD〈3.0%;加样回收率分别为96.81%-102.00%（RSD=1.89%,n=9）、96.64%-102.31%（RSD=1.82%,n=9）。结论：该方法简便、快速、准确,可用于同时测定尼莫地平缓释片中乙醇和丙酮的残留量。
OBJECTIVE： To establish a method for the residual determination of ethanol and acetone in Nimodipine sus- tained-release tablet. METHODS： Headspace GC was on the column of capillary column with fixative solution of 6% cyanopropyl phenyl-94% dimethyl polysiloxane （DB-624） by temperature programming, injector temperature was 230 %, detector was a flame ionization detector, detector temperature was 250 %, carrier gas was nitrogen gas, flow rate was 2.0 ml/min, split ratio was 5 ： 1, equilibrium temperature was 90℃ , equilibrium time was 20 min, and volume of sample was 1.0 ml. RESULTS： The linear range was 1.25-500.0 μg/ml for ethanol （r=0.999 9） and 0.50-202.0 μg/ml for acetone （r=0.999 2）; limits of quantitative were 5.01, 2.02 μg/ml, limits of detection were 1.67, 0.67 μg/ml, respectively; RSDs of precision, stability and reproducibility tests were lower than 3.0% ; recoveries were 96.81% -102.00% （RSD=1.89%, n=9）, 96.64% -102.31% （RSD=1.82%, n=9）, respectively. CONCLUSIONS： The method is simple, rapid, accurate, and can be used for simultaneous residual determination of ethanol and acetone in Nimodipine sustained-release tablet.
出处
《中国药房》
CAS
北大核心
2016年第33期4686-4688,共3页
China Pharmacy
基金
国家自然科学基金资助项目(No.21402012)
国家自然科学项目子项目(No.GJZXM201605)
