摘要
提出了高效液相色谱-电雾式检测器法(HPLC-CAD)测定卡格列净中葡萄糖酸-δ-内酯(GDL)的含量。优化的色谱条件如下:Thermo Hypersil Gold Aq色谱柱(250 mm×4.6 mm,5μm),流动相为乙腈(9+1)混合溶液,流量0.5mL·min^(-1),柱温30℃,进样量10μL;电雾式检测器(CAD)的雾化温度为50℃,载气压力427.5kPa。在上述的色谱条件下,GDL的线性范围为1.05~22.5mg·L^(-1),GDL的检出限(3S/N)为0.32ng。在3个浓度水平上进行加标回收试验,测得回收率在96.2%~103%之间。供试品加标溶液和对照品溶液在室温条件下放置12h内稳定,测定值的相对标准偏差(n=7)分别为1.8%,1.3%。
A method for determination of Glucono-δ-Lactone （GDL） in Canagliflozin was proposed by HPLC coupled with charged aerosol detection （HPLC-CAD）. The optimized chromatographic conditions were as follows： （1） Thermo Hypersil Gold Aq column （250 min×4. 6 mm, 5 μm） was used as stationary phase; （2） the mobile phase was a mixture of acetonitrile-water （9＋1） solution with a flow rate of 0. 5 mL ·min^-1 ; （3） column temperature was 30 ℃; （4） the injection volume was 10μL; （5） the nebulization temperature of CAD was set at 50 ℃, and pressure of carrier gas was 427.5 kPa. Under above chromatographic conditions, linearity range for GDL in mass concentration found was 1.05--22.5 mg · L^-1 , and the detection limit （3S/N） found was 0. 32 ng. Test for recovery was made hy standard addition method at 3 concentration levels, giving results in the range of 96. 2%- 103%. The sample solution and reference solution were stable for 12 h at room temperature, and RSDs （n=7） found were 1.8% and 1.3%, respectively.
出处
《理化检验（化学分册）》
CSCD
北大核心
2017年第4期387-392,共6页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
