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六味安消胶囊的指纹图谱及含量测定

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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。8 μm)，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2 μL。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。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)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。
UPLC fingerprint and quantitative analysis of 10 active components of Liuwei'anxiao capsule
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 0-180.5μg·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 of Liuwei'anxiao capsule and the content determination method for simultaneously detecting the 10 active components are simple,accurate and reliable,which can provide reference for the quality control of Liuwei'anxiao capsule.

Liuwei'anxiao capsuleUPLCUPLC fingerprintscontent determination

曾雪蔚、卫柳辛、张振山、秦国栋、赵春杰

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沈阳药科大学 药学院,辽宁 沈阳 110016

珠海亿胜生物制药有限公司,广东 珠海 519085

广东司法警官职业学院,广东 广州 510520

六味安消胶囊 超高效液相色谱 UPLC指纹图谱 含量测定

2024

10.14066/j.cnki.cn21-1349/r.2023.0612

沈阳药科大学学报
沈阳药科大学

沈阳药科大学学报

CSTPCD
影响因子：0.604
ISSN：1006-2858
年,卷(期)：2024.41(8)