摘要
目的 采用HPLC-UV-ELSD法测定益肝乐颗粒（垂盆草、柴胡、板蓝根等）中槲皮素、山柰素、柴胡皂苷a和柴胡皂苷d的量.方法 Hypersil C18色谱柱（4.6 mm×150 mm,5μm）;体积流量0.8 mL/min;槲皮素和山柰素的检测流动相为甲醇-水-三氟乙酸（40∶60∶0.05）,检测波长360 nm.柴胡皂苷a和柴胡皂苷d的检测流动相为甲醇-乙腈-水（25∶45∶30）,ELSD漂移管温度95℃,载气（N2）体积流量2.4 SLPM/min.结果 槲皮素和山柰素分别在0.071 3～1.426 μg（r=0.999 7）、0.056 8 ～1.136 μg（r=0.999 3）进样量与峰面积呈良好的线性关系,平均加样回收率分别为97.73％、96.97％,RSD（n=6）分别为1.63％、1.52％.柴胡皂苷a和柴胡皂苷d分别在0.041 6～0.8320μg （r=0.9992）、0.026 7 ～0.534 0μg（r=0.999 5）进样量的自然对数值与峰面积的自然对数值呈良好的线性关系,平均加样回收率分别为97.35％、98.04％,RSD （n=6）分别为0.81％、1.16％.结论 该方法测定结果准确、灵敏、重复性好.
AIM To develop an HPLC-UV-ELSD method for determining the content of quercetin, kaempfer- ol, saikosaponin a and saikosaponin d in Yiganle Granules （Sedi Herba, Bupleuri Radix, Isatidis Radix, etc. ）. METHODS An Hypersil Cls column was used as the chromatographic column, the flow rate was 0. 8 mL/min. The mobile phase for quercetin and kaempferol consisted of methanol-water-trifluoroacetic acid （40 ： 60 ： 0.05）. The UV detection wavelength was set at 360 nm. The mobile phase for saikosaponin a and saikosaponin d consisted of methanol-acetonitrile-water （25 ： 45 ： 30）, the temperature of drift tube was set at 95 ℃, and the gas flow （ N2 ） at 2. 4 SLPM/min. RESULTS There was a good linear relationship between the concentration of quercetin, kaempferol and peak area value at the concentrations of 0. 071 3 - 1. 426 μg （r =0. 999 7）, and 0. 056 8 - 1. 136 μg （r =0. 999 3）. The average recovery were 97.73% （RSD = 1.63% ） and 96. 97% （RSD = 1.52% ）, re- spectively. There was a good linear relationship in the concentrations of saikosaponin a and saikosaponin d at the concentration of 0.041 6-0.832 0 μg （r=0.999 2）, 0.026 7 -0.534 0 μg （r=0.999 5）. The average re- coveries were 97.35% （RSD = 0. 81% ） and 98.04% （RSD = 1.16% ）, respectively. CONCLUSION The method is accurate, sensitive, reproducible and can be used in the determination of quercetin, kaempferol, sai- kosaponin a and saikosaponin d in Yiganle Granules.
出处
《中成药》
CAS
CSCD
北大核心
2014年第3期531-535,共5页
Chinese Traditional Patent Medicine
