六味安消胶囊的指纹图谱及含量测定  

UPLC fingerprint and quantitative analysis of 10 active.components of Liuwei′anxiao capsule

作　　者：曾雪蔚 卫柳辛 张振山 秦国栋 赵春杰[1] ZENG Xuewei;WEI Liuxin;ZHANG Zhenshan;QIN Guodong;ZHAO Chunjie(School of Pharmacy,Shenyang Pharmaceutical University,Shenyang 110016,China;Zhuhai Essex Bio-Pharmaceutical Co.,Ltd.,Zhuhai 519085,China;Guangdong Justice Police Vocational College,Guangzhou 510520,China)

机构地区：[1]沈阳药科大学药学院,辽宁沈阳110016 [2]珠海亿胜生物制药有限公司,广东珠海519085 [3]广东司法警官职业学院,广东广州510520

出　　处：《沈阳药科大学学报》2024年第8期1074-1086,共13页Journal of Shenyang Pharmaceutical University

摘　　要：目的采用超高效液相色谱法,建立六味安消胶囊的超高效液相(Ultra High Performance Liquid Phase,UPLC)指纹图谱及10种有效成分(没食子酸、鞣花酸、芦荟大黄素、大黄酸、山奈素、大黄素、大黄酚、大黄素甲醚、土木香内酯、异土木香内酯)的含量测定方法。方法采用超高效液相色谱法,色谱柱为Waters ACQUITY UPLC HSS T3柱(100 mm×2.1 mm,1.8μm),流动相为乙腈-体积分数0.2%的磷酸溶液,梯度洗脱,流速为0.2 mL·min^(-1),柱温为30℃,检测波长为254 nm(指纹图谱)和194 nm,进样量为2μL。结果建立了六味安消胶囊的UPLC指纹图谱,以芦荟大黄素为参照峰,标定了20个共有峰,相似度均大于0.995,并指认了没食子酸、鞣花酸、芦荟大黄素、大黄酸、山奈素、大黄素、大黄酚、大黄素甲醚8个共有峰,聚类分析将10批六味安消胶囊样品聚为2类。定量分析条件方法学考察结果良好,结果显示,没食子酸、鞣花酸、芦荟大黄素、大黄酸、山奈素、大黄素、异土木香内酯、土木香内酯、大黄酚、大黄素甲醚的质量浓度分别在0~180.5μg·mL^(-1)(r=1.0000)、0~173.5μg·mL^(-1)(r=0.9999)、0~48.5μg·mL^(-1)(r=1.0000)、0~55.0μg·mL^(-1)(r=1.0000)、0~188.0μg·mL^(-1)(r=1.0000)、0~62.0μg·mL^(-1)(r=1.0000)、0~65.5μg·mL^(-1)(r=1.0000)、0~131.0μg·mL^(-1)(r=0.9999)、0~91.5μg·mL^(-1)(r=0.9999)、0~31.0μg·mL^(-1)(r=0.9999)内与峰面积成良好的线性关系。平均回收率分别为101.38%、96.07%、98.62%、93.21%、93.58%、97.67%、96.50%、97.68%、96.95%、98.72%,RSD分别为3.21%、3.05%、3.96%、1.03%、2.22%、3.52%、3.72%、3.29%、3.07%、3.60%。结论建立了六味安消胶囊UPLC指纹图谱及同时测定10种有效成分含量的方法,操作简便,准确可靠,为六味安消胶囊的质量控制与评价提供了理论依据。Objective To establish a UPLC method for the fingerprint of Liuwei′anxiao capsule and the content determination of 10 active.components(gallic acid,ellagic acid,aloe-emodin,rhein,kaempferol,emodin,chrysophanol,physcion,alantolactone,isoalantolactone).Methods An UPLC method was developed to establish the fingerprint and determination method.The analysis was carried out using a Waters ACQUITY UPLC HSS T3(100 mm×2.1 mm,1.8 μm) column with a mobile phase of acetonitrile-0.2% phosphoric acid solution with gradient elution.The flow rate was 0.2 mL·min~(-1) and column temperature was 30 ℃.The detection wavelength were 254 nm(fingerprint),194 nm,and the injection volume was 2 μL.Results The UPLC fingerprint of Liuwei′anxiao capsule was established.With aloe-emodin as the reference peak,20.common peaks were identified,the similarity was higher than 0.995.8 peaks confirmedas gallic acid,ellagic acid,aloe-emodin,rhein,kaempferide,emodin,chrysophanol,physcion were confirmed.10 batches of Liuwei′anxiao capsule samples were grouped into 2 categories by cluster analysis.The results of quantitative analysis condition methodology were good.The calibration curves were linear within the range of 0-180.5 μg·mL~(-1)(r=1.000 0)、0-173.5 μg·mL~(-1)(r=0.999 9)、0-48.5 μg·mL~(-1)(r=1.000 0)、0-55.0 μg·mL~(-1)(r=1.000 0)、0-188.0 μg·mL~(-1)(r=1.000 0)、0-62.0 μg·mL~(-1)(r=1.000 0)、0-65.5 μg·mL~(-1)(r=1.000 0)、0-131.0 μg·mL~(-1)(r=0.999 9)、0-91.5 μg·mL~(-1)(r=0.999 9)、0-31.0 μg·mL~(-1)(r=0.999 9) for gallic acid,ellagic acid,aloe-emodin,rhein,kaempferide,emodin,isoalantolactone,alantolactone,chrysophanol and physcion,respectively.The average recoveries were 101.38%,96.07%,98.62%,93.21%,93.58%,97.67%,96.50%,97.68%,96.95% and 98.72% for gallic acid,ellagic acid,aloe-emodin,rhein,kaempferide,emodin,isoalantolactone,alantolactone,chrysophanol and physcion,respectively,with RSD of 3.21%,3.05%,3.96%,1.03%,2.22%,3.52%,3.72%,3.29%,3.07% and 3.60%,respectively.Conclusion The established HPLC fingerprint

关 键 词：六味安消胶囊 超高效液相色谱 UPLC指纹图谱 含量测定 

分 类 号：R917[医药卫生—药物分析学]