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目的:采用高效液相色谱法同时测定牛黄降压丸中芍药苷和黄芩苷的含量。方法:牛黄降压丸用50%乙醇超声提取3次,每次15min。色谱柱为Agilent Zorbax SB-C18(4.6mm×150mm,5μm);流动相:A相为0.1%甲酸-甲醇,B相为0.1%甲酸-水,梯度洗脱(0～8min,30%A;8～10min,30%→39%A;10～30min,39%A);流速:1.0mL·min-1;检测波长:230nm;柱温:30℃;进样量:5μL。结果:芍药苷和黄芩苷的回归方程分别为Y=6.724X+7.063(r=0.9993)和Y=6.744X-102.5(r=0.9990),线性范围分别为6.85～53.5μg·mL-1和106.2～1080μg·mL-1。方法学考察结果表明,芍药苷低、中、高3个浓度点的日内、日间精密度的RSD分别为1.6%,1.2%,1.0%和1.8%,1.8%,1.2%;黄芩苷低、中、高3个浓度点的日内、日间精密度的RSD分别为1.2%,0.43%,0.18%和1.9%,1.1%,0.54%。芍药苷和黄芩苷最低检测限(S/N=3)分别为2.7μg·mL-1和5.4μg·mL-1,加样回收率(n=6)分别为99.57%(RSD=1.5%)和99.76%(RSD=1.3%)。结论:采用高效液相色谱法同时测定牛黄降压丸中芍药苷和黄芩苷的含量,样品处理方法简便,测定结果准确,方法专属性强,精密度高,重复性好。
Objective: To determine the contents of paeoniflorin and baicalin in Niuhuang Jiangya Pills by high performance liquid chromatography (HPLC). Methods: Bezoar antihypertensive pill with 50% ethanol ultrasonic extraction three times, each time 15min. The mobile phase consisted of 0.1% formic acid-methanol in phase A and 0.1% formic acid-water in phase B, gradient elution (0-8 min, 30% A; 8 to 10 min, 30% to 39% A; 10 to 30 min, 39% A); flow rate: 1.0 mL · min-1; detection wavelength: 230 nm; Results: The regression equations of paeoniflorin and baicalin were Y = 6.724X + 7.063 (r = 0.9993) and Y = 6.744X-102.5 (r = 0.9990) respectively. The linear range was from 6.85 to 53.5μg · mL- ~ 1080μg · mL-1. The results of the methodological study showed that the intra-day and inter-day RSDs of paeoniflorin were 1.6%, 1.2%, 1.0% and 1.8%, 1.8% and 1.2%, respectively. The RSDs of intra-day and inter-day precision at the three concentrations were 1.2%, 0.43%, 0.18% and 1.9%, 1.1% and 0.54%, respectively. The detection limits of paeoniflorin and baicalin (S / N = 3) were 2.7μg · mL-1 and 5.4μg · mL-1, respectively. The recovery rates of paeoniflorin and baicalin were 99.57% (RSD = 1.5% And 99.76% (RSD = 1.3%). Conclusion: The content of paeoniflorin and baicalin in Niuhuang Jiangya Pill was determined by HPLC at the same time. The method of sample processing was simple, the method was accurate, the specificity was high, the precision was high and the repeatability was good.