毛细管胶束电动色谱法分离测定中药半枝莲中的7种有效成分

建立了毛细管胶束电动色谱同时分析检测中药半枝莲药材及其膏剂中黄芩素、柚皮素、汉黄芩素、野黄芩苷、芹菜素、木犀草素和原儿茶酸7种有效成分的方法。半枝莲样品中7种有效成分经甲醇超声提取。实验考察了运行缓冲溶液的pH值和浓度、添加剂、检测波长、分离电压和进样时间等重要参数对目标物分离的影响。得到的优化条件为: 运行缓冲液50 mmol/L硼砂-0.20 mol/L硼酸溶液(pH 8.4),含8.5 mmol/L十二烷基硫酸钠(SDS),分离电压25 kV,检测波长260 nm和335 nm。在此条件下,7种组分于12 min内达到基线分离。各组分在8×10~6～3.2×10~4mol/L范围内呈良好的线性关系,相关系数(r2)为0.9965～0.9999;检出限为7.0×10~8～2.0×10~6mol/L;回收率均大于85%。该方法提取简便、准确可靠、重复性好、灵敏度高,可以用于中药半枝莲中7种有效成分的定量检测。

Simultaneous determination of 7 active ingredients in Scutellaria barbata D. Don by capillary micellar electrokinetic chromatography

A method of capillary micellar electrokinetic chromatography with a diode array detector was developed for the simultaneous determination of 7 active ingredients (baicalein, naringenin, wogonin, scutellarin, apigenin, luteolin, and protocatechuic acid) in Scutellaria barbata D. Don and its ointment. The 7 ingredients in samples were extracted with methanol in an ultrasonic bath. The important factors, such as pH, running buffer concentration, additive, detection wavelength, separation voltage and injection time, were optimized. Under the optimum conditions, the 7 analytes were separated within 12 min at a separation voltage of 25 kV in a 50 mmol/L borate-0.20 mol/L boric acid buffer (pH 8.4) containing 8.5 mmol/L sodium dodecyl sulfate (SDS). The detection was carried out at 260 nm and 335 nm. Notably, the linearity ranged from 8×10~6 to 3.2×10~4mol/L with the correlation coefficients (r2) at the range of 0.9965~0.9999. The detection limits (S/N=3) ranged from 7.0×10~8mol/L to 2.0×10~6mol/L for all the 7 analytes. The recoveries of the 7 active ingredients were all over 85%. This method is of good sensitivity, simple preparation, good reproducibility and reliability. It was successfully applied to the analysis of the 7 active ingredients in Scutellaria barbata D. Don and its ointment.