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[摘要]
目的 建立高效液相色谱-蒸发光散射(HPLC-ELSD)法同时测定补血生乳颗粒中的黄芪甲苷、阿魏酸、芍药苷、甘草酸、王不留行黄酮苷、柚皮苷、新橙皮苷、桔梗皂苷D的方法。方法 采用Diamonsil C18色谱柱(250 mm×4.6 mm,5 μm);流动相为0.1%甲酸水溶液-乙腈,梯度洗脱;体积流量1 mL/min;柱温30℃;检测器:ELSD,漂移管温度40℃。结果 各成分在52 min内分离良好,线性范围均为62.5~1 250.0 μg/mL(r>0.995 0);样品各成分平均加样回收率95.51%~99.47%,RSD为0.31%~3.70%;8种成分日内精密度和日间精密度RSD均小于3%;重复性RSD为0.94%~2.11%;供试品溶液在18 h内稳定性良好,RSD在0.98%~2.86%。6批样品中王不留行黄酮苷、芍药苷、阿魏酸、柚皮苷、新橙皮苷、桔梗皂苷D、黄芪甲苷、甘草酸质量分数分别为0.550 7~0.584 3、19.657 9~19.952 1、0.350 5~0.384 7、18.794 7~19.557 3、12.124 7~12.414 2、0.610 7~0.631 3、0.238 8~0.274 3、2.750 4~2.852 2 mg/g。结论 该方法简便、快速、准确,可用于补血生乳颗粒的质量控制。
[Key word]
[Abstract]
Objective To establish an HPLC-ELSD method for simultaneous determination of astragaloside IV, ferulic acid, paeoniflorin, glycyrrhizic acid, vaccarin, naringin, neohesperidin, and platycodin D in Buxue Shengru Granules (BSG). Methods The analysis of methanol extract of this drug was performed on a Diamonsil C18 (250 mm×4.6 mm, 5 μm) with the mobile phase comprising of 0.1% formic acid aqueous solution-acetonitrile. Flow rate was 1 mL/min and column temperature was 30℃. The samples were tested on Evaporative Light-scattering Detector with drift tube temperature of 40℃. Results The analysis permitted very good separation of eight constituents within 52 min. The linearity ranges of the eight constituents were 62.5-1 250.0 μg/mL (r > 0.995 0). The average recoveries of eight constituents in the samples were in the range of 95.51%-99.47%, and the RSD ranged from 0.31% to 3.70%. Intraday and interday precisions RSD of the peak areas of the eight components were less than 3%; The repeatability RSD of each component ranged from 0.94% to 2.11%; Eight components had good stability within 18 h, and the concentration RSD of each component ranged from 0.98% to 2.86%. The content of vaccarin, paeoniflorin, ferulic acid, naringin, neohesperidin, platycodin D, astragaloside IV, and glycyrrhizic acid were 0.550 7-0.584 3, 19.657 9-19.952 1, 0.350 5-0.384 7, 18.794 7-19.557 3, 12.124 7-12.414 2, 0.610 7-0.631 3, 0.238 8-0.274 3, and 2.750 4-2.852 2 mg/g, respectively. Conclusion This simple and accurate method can be used for the rapid quality control of BSG.
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[基金项目]
国家自然科学基金资助项目(21575040);长沙市科技局项目(kc1701009)