目的:建立红毛五加皮中刺五加苷E的定性鉴别和含量测定方法,建立红毛五加皮的质量标准。方法:照2010年版中国药典方法检查红毛五加皮中总灰分和酸不溶性灰分,测定其浸出物含量。采用TLC法鉴别刺五加苷E,薄层色谱使用硅胶G薄层板,以三氯甲烷-甲醇-水(6∶3∶1)的下层溶液为展开剂,10%硫酸乙醇溶液为显色剂;采用HPLC法测定刺五加苷E的含量,色谱柱为Welchrom C18(250 mm×4.6 mm,5μm),流动相为乙腈-0.05%磷酸(13∶87),流速1 mL.min-1,检测波长207 nm,柱温35℃。结果:红毛五加皮中总灰分平均为6.69%,酸不溶性灰分平均为0.71%,浸出物平均含量为15.25%,刺五加苷E薄层斑点清晰,特征明显。刺五加苷E的线性范围为0.02696~1.0784μg(r=1.000),平均加样回收率(n=6)为97.2%(RSD=1.7%)。结论:本文建立的薄层鉴别方法特征明晰,液相色谱方法分离良好,经方法学验证,可用于红毛五加皮药材的质量检测。
Objective:To establish an identification and determination method of eleutheroside E in Cortex Acan- thopanacis Giraldii, and set up the quality standards of Cortex Acanthopanacis Giraldii. Methods:According to 2010 edition of Chinese Pharmacopoeia, the total ash, acid - insoluble ash and extractum were determined. The TLC and HPLC methods were used for qualitative identification and quantitative determination of eleutheroside E. TLC meth- od used silica gel G as the coating substance, underlayer of chloroform -methanol -water(6:3:1 )as the developing solvent, 10% sulfuric acid alcohol solution as coloration. HPLC method was performed on a welchrom Cxs column ( 250 mm× 4.6 mm,5μm) , using the mobile phase of acetonitrile - 0. 05 % phosphonic acid water solution ( 13: 87 ) with a flow rate at 1 mL .min ^- 1, the detection wavelength was set at 207 nm and column temperature was 35 ℃. Results:The average content of total ash and acid -insoluble ash were 6.69% and 0. 71% ,the extractum content was 15.25% on average. The TLC identification was highly specific and spot of eleutheroside E was clear. The line- ar range of eleutheroside E was between 0. 02696 - 1. 0784 μg( r = 1. 000), and the average recovery was 97.2% with RSD 1.7% (n =6). Conclusion:The established TLC and HPLC methods can be used for the quality control of Cortex Acanthopanacis Giraldii.