摘要
目的 建立同时测定栀子大黄汤水提液中15种化学成分含量测定的方法,并考察单煎合冲与合煎对15种成分溶出量的影响。方法 采用UPLC法,色谱柱为Acquity UPLC BEH(2.1 mm×100 mm, i.d.=1.7μm),流动相为乙腈-0.5%甲酸水溶液梯度洗脱,检测波长为254 nm[京尼平龙胆二糖苷(genipin 1-gentiobioside, G1)、京尼平苷(geniposide, G2)、大豆苷、大豆苷元、染料木素]、283 nm(芸香柚皮苷、柚皮苷、橙皮苷、新橙皮苷)、440 nm(西红花苷I、藏红花酸、大黄酸、大黄素、大黄酚、大黄素甲醚),柱温35℃,流速0.3 mL/min,进样量为1μL,采用化学计量学方法分析在单煎合冲与合煎条件下栀子大黄汤15种化学成分溶出量的变化。结果 G1、G2、大豆苷、大豆苷元、染料木素、芸香柚皮苷、柚皮苷、橙皮苷、新橙皮苷、西红花苷I、藏红花酸、大黄酸、大黄素、大黄酚、大黄素甲醚分别在21.56~1 380.00μg/mL(R^(2)=0.999 8)、69.22~4 430.00μg/mL(R^(2)=0.999 6)、1.01~64.50μg/mL(R^(2)=0.999 8)、0.64~41.08μg/mL(R^(2)=0.999 8)、0.61~39.28μg/mL(R^(2)=0.999 8)、8.03~514.00μg/mL(R^(2)=0.999 8)、70.63~2 260.00μg/mL(R^(2)=0.999 1)、12.72~814.00μg/mL(R2=0.999 6)、57.81~1 387.50μg/mL(R^(2)=0.999 2)、5.94~380.00μg/mL(R^(2)=1.000 0)、0.02~1.50μg/mL(R^(2)=0.999 8)、1.11~71.00μg/mL(R^(2)=0.999 6)、0.19~12.45μg/mL(R^(2)=0.999 9)、0.10~6.64μg/mL(R^(2)=0.999 9)和0.03~1.66μg/mL(R^(2)=0.999 8)线性范围内关系良好。等体积合冲样品中柚皮苷、新橙皮苷、大豆苷、大豆苷元、染料木素、大黄素、大黄酚、大黄素甲醚、藏红花酸等9个成分的溶出含量较栀子大黄汤合煎样品显著提高,增高达到12%以上,尤以对含量较低成分如大黄素、大黄酚、大黄素甲醚等溶出增加显著,溶出达50%以上;而对于栀子大黄汤中含量最高的G2,含量居中的G1、橙皮苷、芸香柚皮苷、藏红花素等成分,溶出量变化不大,变化波动在±5%,差异较小。结论 栀子大黄汤复方合煎与单煎合冲样品在化学成分种类上未见明显差异,对含量较低的成分,等体积有利于其溶出。可为复方制剂与单味药配方颗粒制剂的临床合理应用与评价提供参考依据。
Objective To establish a method for the simultaneous determination of 15 chemical components in the water extract of Zhizi Dahuang Decoction(栀子大黄汤)and investigate the effects of single decoction mixture and combined decoction on the dissolution of 15 components.s Methods The chromatographic column was Acquity UPLC BEH(2.1 mm×100 mm,i.d.=1.7μm).The mobile phase was gradient eluted with acetonitrile-0.5%formic acid aqueous solution.The detection wavelength was 254 nm[genipin 1-gentiobioside(G1),geniposide(G2),daidzin,daidzein,genistein],283 nm(rutin,naringin,hesperidin,neohesperidin),440 nm(crocin I,saffron,rhein,emodin,chrysophanol,and emodin methyl ether).The column temperature was 35℃,the flow rate was 0.3 mL/min,and the injection volume was 1μL.Chemometrics method was used to analyze the dissolu-tion of 15 components in Zhizi Dahuang Decoction under the conditions of single decoction and combined decoction.s Results G1,G2,daidzin,daidzein,genistein,naringin,naringin,hesperidin,neohesperidin,crocin I,crocetin,rhein,emodin,chrysophanol and emodin methyl ether were 21.56~1380.00μg/mL(R^(2)=0.9998),69.22~4430.00μg/mL(R^(2)=0.9996),1.01~64.50μg/mL(R^(2)=0.9998),0.64~41.08μg/mL(R^(2)=0.9998),0.61~39.28μg/mL(R^(2)=0.9998),8.03~514.00μg/mL(R^(2)=0.9998),70.63~2260.00μg/mL(R^(2)=0.9991),12.72~814.00μg/mL(R^(2)=0.9996),57.81~1387.50μg/mL(R^(2)=0.9992),5.94~380.00μg/mL(R^(2)=1.0000),0.02~1.50μg/mL(R^(2)=0.9998),1.11~71.00μg/mL(R^(2)=0.9996),0.19~12.45μg/mL(R^(2)=0.9999),0.10~6.64μg/mL(R^(2)=0.9999)and 0.03~1.66μg/mL(R^(2)=0.9998),respectively.The linear range of was good.The dissolution contents of naringin,neohesperidin,daidzein,daidzein,genistein,emo-din,chrysophanol,emodin methyl ether and saffron acid in the equal volume of single decoction mixture was significantly higher than that in the combined decoction of Zhizi Dahuang Decoction,with an increase of more than 12%,especially for the lower con-tent components such as emodin,chrysophanol and emodin methyl ether,with a dissolution of more than 50%.However,for G2 with the highest content in Zhizi Dahuang Decoction and G1,hesperidin,rutin,saffron and other components with the middle con-tents,the dissolution amount had little change,with a fluctuation of±5%.n Conclusion There is no significant difference in the chemical components between the combined decoction and the single decoction mixture of Zhizi Dahuang Decoction.For the com-ponents with low contents,the equal volume is conducive to their dissolution.It can provide a reference for the clinical rational application and evaluation of compound preparations and single drug granules.
作者
王云
张雪
夏梦雨
吴宏伟
杨洪军
张村
WANG Yun;ZHANG Xue;XIA Mengyu;WU Hongwei;YANG Hongjun;ZHANG Cun(Institute of Chinese Materia Medica,China Academy of Chinese Medical Sciences,Beijing 100700,China;College of Pharmacy,Henan University of Chinese Medicine,Zhengzhou 450008,Henan,China;Experiment research center,China Academy of Chinese Medical Sciences,Beijing 100700,China)
出处
《中华中医药学刊》
CAS
北大核心
2023年第10期53-59,I0011,I0012,共9页
Chinese Archives of Traditional Chinese Medicine
基金
国家自然科学基金项目(81873010,81703708)
中央级公益性科研院所基本科研业务项目(ZZ13-019,ZXKT17044)。
关键词
栀子大黄汤
合煎
合冲
超高效液相色谱法
等体积
等倍量
含量测定
物质基础
Zhizi Dahuang Decoction(栀子大黄汤)
combined decoction
mixture of single decoction
UPLC
equal volume
equal multiple
content assay
material basis
