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.
[1] 赵天才,杨景锋.甘姜苓术汤治疗肾着病浅见[J].中医学报,2015,30(5):660
ZHAO TC,YANG JF.Gan Jiang Ling Zhu Tang in the treatment of affection of kidney by cold-dampness[J].China J Chin Med, 2015,30(5):660
[2] 李其香,黄宗菊.甘姜苓术汤加减治疗慢性盆腔炎性痛经疗效观察[J].实用中医药杂志,2018,34(8):892
li qx,huang zj.observation of curative effect of ganjianglingzhu decoction on chronic pelvic inflammatory dysmenorrhea[j].j pract tradit chin med,2018,34(8):892
[3] 李璇,刘春芳.肾着汤治疗肾积水 1 例[J].实用中医药杂志,2018,34(2):26
LI X,LIU CF.Shenzhu decoction for hydronephrosis:a case report[J].J Pract Tradit Chin Med,2018,34(2):26
[4] 李金城,王培歌.甘姜苓术汤治疗膝骨关节炎[J].中医药临床杂志,2017,29(8):1170
LI JC,WANG PG.Discussion on Ganjiang Lingzhu decoction in the treatment of knee osteoarthritis[J].J Pract Tradit Chin Med,2017, 29(8):1170
[5] 倪珊珊,王耀光.王耀光运用甘姜苓术汤治疗冷淋 1 例[J].江西中医药,2013,44(2):14
NI SS,WANG YG.Wang Yaoguang used Ganjianglingzhu decoction to treat a cold shower[J].Jiangxi J Tradit Chin Med,2013,44(2): 14
[6] 张玉姗,刘谢英,姚新成,等.高效液相色谱法同时测定茵栀黄颗粒中 14 个化学成分[J].药物分析杂志,2019,39(7):1229
ZHANG YS,LIU XY,YAO XC,et al.Simultaneous determination of fourteen constituents in Yinzhihuang granules by HPLC[J].Chin J Pharm Anal,2019,39(7):1229
[7] 魏晓萌,严华,陆以云,等.HPLC 法同时测定锥叶柴胡中 6 个主要皂苷类成分的含量[J].药物分析杂志,2018,38(4):618
WEI XM,YAN H,LU YY,et al .HPLC simultaneous determination of 6 main saponins in Bupleurum bicaule Helm.[J].Chin J Pharm Anal,2018,38(4):618
[8] 周恒,曹依敏,苗水,等.HPLC 法测定沪地龙中 7 个核苷类成分的含量[J].药物分析杂志,2018,38(1):97
ZHOU H,CHAO YM,MIAO S,et al.Determination of 7 nucleosides in Shanghai Pheretima by HPLC[J].Chin J Pharm Anal,2018,38(1):97
[9] 阚艳红. 消栓肠溶胶囊的 HPLC 指纹图谱及 5 个活性成分的测定[J].药物分析杂志,2019,39(5):937
GAN YH.HPLC fingerprint of Xiaoshuan enteric-coated caplsules and determination of five active components[J].Chin J Pharm Anal,2019,39(5):937
[10] 于小红,吴昊,赵奎君,等.柴胡桂枝汤高效液相色谱指纹图谱的建立[J].药物分析杂志,2019,39(7):1249
YU XH,WU H,ZHAO KJ,et al.Establishment of HPLC fingerprint of Chaihu Guizhi decoction[J].Chin J Pharm Anal,2019,39(7): 1249
[11] LI WF,JIANG JG,CHEN J.Chinese medicine and its modernization demands[J].Arch Med Res,2008,39(2):246
[12] WANG Y,KONG L,HU L,et al.Biological fingerprinting analysis of the traditional Chinese prescription Longdan Xiegan decoction by on/off-line comprehensive two-dimensional biochromatography[J]. J Chromatogr B Anal Technol Biomed Life Sci,2007,860(2):185
[13] 中华人民共和国药典 2015 年版.一部华人民共和国药典 2015 年版.一部[S].2015:86 ChP 2015.Vol Ⅰ[S].2015:86
[14] 金辉,司昕蕾,边甜甜,等.不同产地甘草的 HPLC 指纹图谱研究[J].中兽医医药杂志,2018,37(4):49
JIN H,SI XL,BIAN TT,et al.HPLC fingerprinting analysis of Radix Glycyrrhizae[J].J Tradit Chin Vet Med,2018,37(4):49
[15] 伍蕊嗣,姚运秀,刘钱,等.不同干燥方式泽泻汤指纹图谱的建立及 2 种成分测定[J].中成药,2019,41(8):1905
WU RS,YAO YX,LIU Q,et al.Establishment of fingerprints of alisma decoction with different drying methods and determination of two constituents[J].Chin Tradit Pat Med,2019,41(8):1905
[16] 刘艳,章军,陈士林,等.经典名方复方制剂研发策略[J].中国实验方剂学杂志,2019,25(24):166
LIU Y,ZHNAG J,CHEN SL,et al.Research and development strategy of classical formula compound preparation[J].Chin J Exp Tradit Med Form,2019,25(24):166
[17] 高喜梅,贾萌,赵晓莉,等.经典名方传统制法向现代生产工艺转化关键问题探索[J].南京中医药大学学报,2019,35(5):601
GAO XM,JIA M,ZHAO XL,et al.Exploration on the key problems in the transformation from traditional preparation to modern manufacture of classical famous prescriptions[J].J Nanjing Univ Tradit Chin Med,2019,35(5):601
[18] 张倩,韩星星,毛春芹,等.中药复方制剂开发的机遇与挑战:古代经典名方研究开发的问题分析[J].中国中药杂志,2019,44(19):4300
ZHANG Q,HAN XX,MAO CQ,et al.Opportunities and challenges in development of compound preparations of traditional Chinese medicine:problems and countermeasures in research of ancient classical prescriptions[J].China J Chin Mater Med,2019,44(19): 4300
