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.
作者
刘鹤
贺丹彤
邢春来
何蕊
贾艾玲
杨净尧
刘睿
邱智东
位鸿
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)
出处
《药物分析杂志》
CAS
CSCD
北大核心
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)。
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
classic famous prescription
Ganjianglingzhu decoction
corresponding object quality control
fingerprint
glycyrrhizin
ammonium glycyrrhetate
6-gingerol
