甘姜苓术汤HPLC指纹图谱及含量测定方法的建立  

Establishment of HPLC fingerprint and content determination method of Ganjianglingzhu decoction

作　　者：刘鹤[1] 贺丹彤 邢春来 何蕊[2] 贾艾玲[1] 杨净尧 刘睿[1] 邱智东[1] 位鸿[2] LIU He;HE Dan-tong;XING Chun-lai;HE Rui;JIA Ai-ling;YANG Jing-yao;LIU Rui;QIU Zhi-dong;WEI Hong(Changchun University of Traditional Chinese Medicine,Changchun 130117,China;Affiliated Hospital of Changchun University of Traditional Chinese Medicine,Changchun 130021,China)

机构地区：[1]长春中医药大学,长春130117 [2]长春中医药大学附属医院,长春130021

出　　处：《药物分析杂志》2021年第1期42-50,共9页Chinese Journal of Pharmaceutical Analysis

基　　金：吉林省科技发展计划项目(No.20190304077YY)。

摘　　要：目的:制备甘姜苓术汤对应实物,建立适用于甘姜苓术汤对应实物HPLC含量测定以及指纹图谱方法。方法:依照古籍记载制备甘姜苓术汤对应实物;应用HPLC对15批对应实物进行有效成分含量测定和指纹图谱建立,流动相为乙腈-0.05%磷酸水,梯度洗脱,检测波长237 nm。结果:建立甘姜苓术汤的HPLC含量测定和指纹图谱的分析方法,甘草苷、甘草酸、6-姜辣素的专属性试验中峰分离度均大于1.5;精密度试验的RSD分别为0.74%、0.65%、0.69%;重复性试验的RSD分别为1.1%、0.86%、0.92%;稳定性试验RSD分别为0.43%、0.78%、3.0%;回收率分别为99.7%、104.5%、95.1%。在对应实物指纹图谱中以甘草苷峰为参照峰,确定了15个共有峰,通过对照品比对,指认出4号峰为甘草苷,13号峰为甘草酸,14号峰为6-姜辣素,对应实物指纹图谱与对照指纹图谱相似度良好,均大于0.9。15批物质基准对应实物指标成分甘草苷、甘草酸、6-姜辣素的平均含量分别为24.5、35.6、1.6 mg·g^(-1)。结论:建立的经典名方甘姜苓术汤指纹图谱及3个成分的含量测定方法简便,准确可靠,可用于甘姜苓术汤物质基准的质量控制。Objective:To prepare the corresponding physical products of Ganjiang Lingshu decoction,in order to establish a method for HPLC content determination and fingerprinting of the corresponding physical products of Ganjiang Lingzhu decoction.Methods:According to the ancient books,Ganjianglingzhu decoction was prepared,the contents of active components and fingerprint of 15 corresponding materials were established by HPLC,the mobile phase was eluted with acetonitrile-0.05%phosphate water gradient,and the detection wavelength was 237 nm.Results:The HPLC content determination and fingerprint analysis method of Ganjiang Lingshu decoction was established.The peak resolutions in the specificity test of glycyrrhizin,glycyrrhizic acid and 6-gingerol were all greater than 1.5;the RSDs of the precision test were 0.74%,0.65%,and 0.69%respectively;the RSDs of the repeatability test were 1.1%,0.86%,0.92%;the RSDs of the stability test were 0.43%,0.78%,and 3.0%;the recoveries were 99.7%,104.5%,and 95.1%,respectively.In the fingerprint of the corresponding physical product,glycyrrhizin was used as the reference peak,and 15 common peaks were determined.By comparison with the reference substance,it was identified that peak 4 was glycyrrhizin,peak 13 was glycyrrhizin,and peak 14 was 6-ginger.The similarity between the corresponding physical fingerprint and the control fingerprint was good,and both were greater than 0.9.The average content of glycyrrhizin,glycyrrhizic acid,and 6-gingerol in 15 batches of material standards was 24.5,35.6,and 1.6 mg·g^(-1),respectively.Conclusion:The established fingerprint of Ganjianglingshu decoction and the content determination method for detecting the three components are simple,accurate and reliable,and can be used for quality control of its material standards.

关 键 词：经典名方 甘姜苓术汤 对应实物 质量控制 指纹图谱 甘草苷 甘草酸铵 6-姜辣素 

分 类 号：R917[医药卫生—药物分析学]