复方双花片指纹图谱分析及多指标成分含量测定  

Fingerprint Analysis of Compound Shuanghua Tablets and Content Determination of Multi-Index Components

作　　者：曾锦燕 叶绿萍[1] 甘静玉 ZENG Jinyan;YE Lyuping;GAN Jingyu(The First Affiliated Hospital of Guangxi University of Chinese Medicine,Nanning,Guangxi,China 530023)

机构地区：[1]广西中医药大学第一附属医院,广西南宁530023

出　　处：《中国药业》2024年第18期66-70,共5页China Pharmaceuticals

摘　　要：目的建立复方双花片指纹图谱并结合化学模式评价质量。方法采用高效液相色谱(HPLC)法,色谱柱为Shimadzu Wondasil C18柱(250 mm×4.6 mm,5μm),流动相为乙腈-0.05%磷酸水溶液(梯度洗脱),流速为1.0 mL/min,检测波长0~20 min时为278 nm、20~45 min时为330 nm、45~75 min时为278 nm,柱温为30℃,进样量为20μL,建立10批样品的指纹图谱,采用中药色谱指纹图谱相似度评价系统(2012A版)进行相似度评价,确定共有峰;采用偏最小二乘判别分析(PLS-DA)技术分析共有峰化学模式,筛选差异性标志物,测定含量。结果建立的指纹图谱共标定23个共有峰;10批样品相似度均大于0.950;共筛选出8个差异性标志物。(R,S)-告依春、绿原酸、咖啡酸、木犀草苷、穿心莲内酯、连翘苷、槲皮素、脱水穿心莲内酯质量浓度分别在12.74~127.42μg/mL、223.98~2239.78μg/mL、25.83~258.33μg/mL、17.42~174.19μg/mL、10.05~100.54μg/mL、20.48~204.84μg/mL、32.66~326.61μg/mL、18.63~186.29μg/mL范围内与峰面积线性关系良好(r>0.9980,n=6);精密度、稳定性、重复性试验结果的RSD均小于2.0%;平均加样回收率分别为101.37%,100.08%,99.36%,102.31%,101.18%,98.46%,99.09%,102.34%,RSD分别为1.39%,2.52%,1.69%,2.22%,2.31%,1.88%,1.64%,1.72%(n=6)。结论所建立的方法简便快速、稳定可行、专属性强,结果准确可靠,可用于复方双花片的质量评价。Objective To establish the fingerprint of Compound Shuanghua Tablets and evaluate their quality based on the chemical pattern analysis.Methods The high-performance liquid chromatography(HPLC)method was adopted.The chromatographic column was the Shimadzu Wondasil C18 column(250 mm×4.6 mm,5μm),the mobile phase was acetonitrile-0.05%phosphoric acid aqueous solution(gradient elution),the flow rate was 1.0 mL/min,multiple wavelengths were adopted(278 nm at 0-20 min,330 nm at 20-45 min,278 nm at 45-75 min),the column temperature was 30℃,and the injection volume was 20μL.The fingerprint of 10 batches of samples was established,the Similarity Evaluation System for Chromatographic Fingerprint of Traditional Chinese Medicine(Version 2012A)was used for similarity evaluation,and the common peaks were marked.The partial least squares-discriminant analysis(PLS-DA)method was used to analyze the chemical patterns of common peaks,the differential biomarkers were screened,and their contents were determined.Results A total of 23 common peaks were marked in the fingerprint.The similarity of 10 batches of samples was greater than 0.950.Eight differential biomarkers were screened.The linear ranges of(R,S)-goitrin,chlorogenic acid,caffeic acid,galuteolin,andrographolide,phillyrin,quercetin,and dehydroandrographolide were 12.74-127.42μg/mL,223.98-2239.78μg/mL,25.83-258.33μg/mL,17.42-174.19μg/mL,10.05-100.54μg/mL,20.48-204.84μg/mL,32.66-326.61μg/mL,18.63-186.29μg/mL(r>0.9980,n=6)respectively.The RSDs of precision,stability and repeatability tests were all lower than 2.0%.The average recovery rates of the above eight biomarkers were 101.37%,100.08%,99.36%,102.31%,101.18%,98.46%,99.09%,102.34%with RSDs of 1.39%,2.52%,1.69%,2.22%,2.31%,1.88%,1.64%,1.72%(n=6)respectively.Conclusion The established method is simple,fast,stable,feasible,specific,accurate and reliable,which can be used for the quality evaluation of Compound Shuanghua Tablets.

关 键 词：复方双花片 高效液相色谱法 指纹图谱 相似度评价 化学模式分析 含量测定 

分 类 号：R917[医药卫生—药物分析学] R927[医药卫生—药学]