反相离子对色谱法测定环黄杨碱D的含量

Determination of Cyclobuxine D by Ion-pairing RP-HPLC

建立环黄杨碱D含量测定的反相离子对色谱法。色谱柱Xtimate C_(18)(250 mm×4.6 mm, 5.0μm),以[0.01 mol·L^(-1)磷酸二氢钾溶液与0.01 mol·L^(-1)庚烷磺酸钠溶液等量混合(含有0.2%的三乙胺,使用磷酸调节pH值至3.5)]-乙腈(78∶22,V/V)作为流动相,流速1.0 mL·min^(-1),检测波长208 nm,柱温35℃。环黄杨碱D平均回收率(n=6)结果为100.6%,RSD为0.88%;检测限和定量限分别为0.030μg、0.080μg。本法结果准确,重复性良好,可用于环黄杨碱D含量测定。

An ion-pairing reversed-phase high performance liquid chromatography(RP-HPLC)method for determination of the concentration of cyclobuxine D in active pharmaceutical ingredient(API)was established.RP-HPLC was performed on an Xtimate C_(18) chromatographic(4.6 mm×250 mm,5.0μm)column.The mixed solution(a mixture of equal volume of 0.01 mol·L-1 potassium dihydrogen phosphate solution and 0.01 mol·L^(-1 )solution of sodium heptanesulfonate solution,containing 0.2%triethylamine and finally adjusted to pH 3.5 with phosphoric acid)-acetonitrile(78∶22,V/V)as the mobile phase.The flow rate was 1.0 mL·min^(-1),the detection wavelength was at 208 nm,and the column temperature was 35℃.The average recoveries(n=6)of the cyclobuxine D was 100.6%with RSD was 0.88%.Limits of quantity and detection were 0.030μg and 0.080μg,respectively.This method with good accuracy and repeatability can be used for the determination of content of cyclobuxine D.