生物分配胶束色谱法同时测定清火栀麦片中3种有效成分

目的:建立采用生物分配胶束色谱法同时测定清火栀麦片中栀子苷、穿心莲内酯和脱水穿心莲内酯3种有效成分含量。方法:采用Ultimate AQ-C₁₈(4.6 mm×150 mm,5 μm)色谱柱,以0.04 mol·L^-1 Brij 35水溶液[含0.02 mol·L^-1磷酸二氢钠溶液、0.02 mol·L^-1磷酸氢二钠缓冲液(pH 7.4)、9.2 g·L^-1氯化钠溶液]为流动相,流速1.0 mL·min^-1,检测波长238 nm,柱温37 ℃。结果:栀子苷、穿心莲内酯和脱水穿心莲内酯质量浓度分别在28.0~448、6.80~109及18.0~288 μg·mL^-1范围内有良好的线性关系;平均加样回收率(n=5)分别为98.6%、95.8%和102.7%,RSD分别为1.2%,1.3%和0.95%;3批样品中栀子苷、穿心莲内酯和脱水穿心莲内酯含量分别为4.023~4.214、0.628~0.920和3.471~3.612 mg·g^-1。结论:本方法简便、灵敏,重复性好,经方法学验证,可用于清火栀麦片的质量控制。

Objective:To simultaneously determine the three effective compounds such as geniposide,andrographolide and dehydroandrographolide in Qinghuozhimai tablets by biopartitioning micellar chromatography.Methods:The experiments were carried out using an Ultimate AQ-C₁₈(4.6 mm×150 mm,5 μm)column with gradient elution.The mobile phase consisted of 0.04 mol·L^-1 Brij 35[0.02 mol·L^-1 sodium dihydrogen phosphate,0.02 mol·L^-1 disodium hydrogen phosphate(pH 7.4)and 9.2 g·L^-1 sodium chloride]at a flow rate of 1.0 mL·min^-1,the detection wavelength was 238 nm,and the column temperature was 37 ℃.Results:Under above conditions,geniposide,andrographolide and dehydroandrographolide were completely separated with good linearity.The linear ranges of geniposide,andrographolide and dehydroandrographolide were 28.0~448 μg·mL^-1, 6.80~109 μg·mL^-1 and 18.0~288 μg·mL^-1,respectively.The average reaoveries(n=5)were 98.6%(RSD=1.2%),95.8%(RSD=1.3%)and 102.7%(RSD=0.95%),respectively.The contents of the three components were 4.023~4.217 mg·g^-1,0.628~0.920 mg·g^-1 and 3.471~3.612 mg·g^-1,respectively.Conclusion:The results of this study indicated that the established method is simple,highly sensitive,reproducible,and the methodology validation proved that it can be used for the determination of three effective components in Qinghuozhimai tablets production.