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    高效液相色谱法测定卡格列净中葡萄糖酸-δ-内酯的含量

    HPLC Determination of Glucono-δ-Lactone in Canagliflozin

    • 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,5 μm),流动相为乙腈(9+1)混合溶液,流量0.5 mL·min-1,柱温30 ℃,进样量10 μL;电雾式检测器(CAD)的雾化温度为50 ℃,载气压力427.5 kPa。在上述的色谱条件下,GDL的线性范围为1.05~22.5 mg·L-1,GDL的检出限(3S/N)为0.32 ng。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12 h内稳定,测定值的相对标准偏差(n=7)分别为1.8%,1.3%。

       

      Abstract: 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 mm×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 10 μL; 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 by 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.

       

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