饱和流出式固相萃取法测定黄连上清丸中小檗碱的含量

Saturated flow-through mode in SPE to determine berberine in Huanglian Shangqing pills by HPLC-UV

目的:建立一种简便快速、准确可靠的除去黄连上清丸大量基质而测定其指标成分小檗碱的样品前处理方法。方法:样品溶解过滤后的滤液在重力的作用下持续流经氧化铝固相萃取小柱,固相萃取小柱吸附溶液中大量的基质而小檗碱在柱子上快速达到吸附平衡后以恒定的浓度流出小柱;在一定的时间段收集该流出液作为含量测定的供试品溶液,该供试品溶液注入高效液相色谱仪中进行含量测定,采用 C_(18)色谱柱(4.6 mm×150 mm,5 μm);流动相:0.033 mol·L^(-1)磷酸二氢钾溶液-乙腈(65:35);流速:1.0 mL·min^(-1);检测波长:424 nm。结果:收集液中小檗碱的浓度与流经固相萃取小柱前溶液的浓度相等而基质信号大大降低。结论:该法简单快速,可用于以小檗碱为指标成分的中药含量测定。

Objective： To establish a simplified, accurate and rapid method to determine the bulk matrix of the solution for content measurement of the berberine in Huanglian Shangqing pills. Method：The dissolved and filtered sample solutions were persistendy passed through the small columns packed with basic alumina by the self gravity, the bulk matrix was held down by the alumina and hint to elute out while berberine reached a absorption - adsorption equilibrium immediately and eluted out with a constant concentration. The collected solutions at a specified time window were injected into an HPLC system to measure the concentration of the berberine. The measurements were carried out with the reversed phase Cls column（4. 6 mm ×150 mm,5μm） ,the mobile phase was 0. 033 mol·L^-1 KH2P04 - CH3CN（65： 35） at the flow rate of 1.0 mL· min^-1, the detect wavelength was set at 424 nm. Results：The concentration of berberine in the eluted solution at a specified time window was equal to that of berberine before the sample solutions were passed through the columns while the matrix signals were intensively reduced. Conclusion：The method is simple, rapid, and accurate and can be used for the determination of berberine in Chinese patent medicines.