小蓟饮片标准煎液中蒙花苷的TLC鉴别及HPLC含量测定

Identification and determination of linarin in standard decoction of Cirsium setosum by TLC and HPLC

目的建立小蓟标准煎液中蒙花苷的TLC鉴别及HPLC含量测定的方法。方法采用TLC法对小蓟标准煎液进行定性鉴别,以乙酰丙酮-丁酮-乙醇-水(体积比1∶3∶3∶13)为展开剂,AlCl_3试液为显色剂;采用HPLC法测定不同厂家不同批次小蓟中蒙花苷的含量,Kromasil 100-5C_(18)(250 mm×4.6 mm,5μm)为色谱柱,甲醇-体积分数0.5%醋酸(体积比55∶45)为流动相,流速为1 mL/min,检测波长为326 nm,柱温30℃;并对标准煎液中蒙花苷转移率进行研究。结果 TLC法能鉴别出蒙花苷,且特征斑点清晰,专属性强;HPLC含量测定方法中,蒙花苷在0.11~2.2μg之间与峰面积线性关系良好,r=0.999 9,平均回收率为99.55%(n=6),RSD值为1.9%。15批次小蓟饮片制成的标准煎液中蒙花苷质量浓度为1.03~1.31mg/mL,转移率为76.34%~88.29%。结论所建立的TLC和HPLC法操作简便、准确、重复性好,可以用于小蓟标准煎液的质量控制。

Objective To establish an effective TLC and HPLC method for qualitative and quantitative analysis of standard decoction of Cirsium setosum（ Willd.） MB. Methods TLC was applied for quality analysis with acetylacetone-butanone-ethanol-water（ 1 ∶3 ∶ 3 ∶ 13） as the mobile phase and alchlor solution as the chromogenic agent. The content of linarin was determined by HPLC. The separation was carried out on a Kromasil 100-5C18（ 250 mm× 4.6 mm,5 μm） with methanol-0.5% acetic acid（ 55 ∶45） as the mobile phase for isocratic elution at a flow rate of 1.0 m L/min. The detection wavelength was at 326 nm,and the column temperature was at 30 ℃. Besides,the transfer rate of Linarin was also calculated. Results Linarin could be identified by TLC. The characteristic spots in TLC identification were clear and strongly specific.Linarin showed a good liner relationship in a range of 0.11-2.2 μg,r = 0.999 9. The average recovery was99.55%,and RSD was 1.9%. The content of Linarin in 15 batches of standard decoction of C. setosum was among 1.03-1.31 mg/m L,and the transfer rate was 76.34%-88.29%. Conclusion This method is easy and reliable,and it could be used for the quality control of standard decoction of C. setosum.