[关键词]
[摘要]
目的 建立同时测定龙砂颗粒中黄柏碱、芦丁、黄芩苷、黄芩素、盐酸小檗碱、槲皮素、苍术素7种成分的RP-HPLC方法.方法 采用全时段双波长RP-HPLC,Kromasil C18色谱柱(250 mm×4.6 mm,5 μm);流动相为乙腈 -0.02%磷酸水溶液,梯度洗脱;体积流量1.0 mL/min;柱温30 ℃;检测波长为205 nm(黄柏碱、芦丁、黄芩苷、黄芩素、槲皮素)和340 nm(盐酸小檗碱、苍术素).结果 黄柏碱、芦丁、黄芩苷、黄芩素、盐酸小檗碱、槲皮素、苍术素分别在0.011~0.168 mg/mL(r=0.999 9),0.010~0.160 mg/mL(r=0.999 9),0.053~0.842 mg/mL(r=0.999 9),0.014~0.228 mg/mL(r=0.999 8),0.016~0.266 mg/mL(r=0.999 8),0.009~0.144 mg/mL(r=0.999 9),0.002~0.024 mg/mL(r=0.999 7)线性关系良好,平均加样回收率分别为99.83%、100.09%、99.98%、99.54%、100.14%、99.67%、100.06%,RSD分别为1.9%、2.6%、3.7%、2.4%、2.1%、1.8%、3.2%.结论 该方法简便、准确、重复性好,可用于龙砂颗粒的质量控制.
[Key word]
[Abstract]
Objective To establish the RP-HPLC method for the simultaneous determination of phellodendrine, rutin, baicalin, baicalein, berberine hydrochloride, quercetin, and atractylodin in Longsha Granules. Methods The seven components were measured on a C18 column (250 mm × 4.6 mm, 5 μm) of Kromasil with a gradient elution of acetonitrile-0.02% phosphoric acidsolution at the wavelengths of 205 nm (phellodendrine, rutin, baicalin, baicalein, and quercetin) and 340 nm (berberine hydrochloride and atractylodin), a flow rate of 1.0 mL/min, and the column temperature of 30 ℃. Results Phellodendrine, rutin, baicalin, baicalein, berberine hydrochloride, quercetin, and atractylodin showed a good correlation in the ranges of 0.011-0.168 mg/mL (r = 0.999 9), 0.010-0.160 mg/mL (r = 0.999 9), 0.053-0.842 mg/mL (r = 0.999 9), 0.014-0.228 mg/mL (r = 0.999 8), 0.016-0.266 mg/mL (r = 0.999 8), 0.009-0.144 mg/mL (r = 0.999 9), and 0.002-0.024 mg/mL (r = 0.999 7). The average recovery rates were 99.83%, 100.09%, 99.98%, 99.54%, 100.14%, 99.67%, and 100.06%. The RSD were 1.9%, 2.6%, 3.7%, 2.4%, 2.1%, 1.8%, and 3.2%. Conclusion The method is simple, accurate, and excellent repetition, and can be used to control the quality of Longsha Granules.
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[基金项目]
国家"十二五"科技支撑计划项目(2012BA127B07);四川省科技厅科技支撑项目(2011SZ0071)