HPLC同时测定不同厂家丹七片中多个有效成分的含量  

Simultaneous determination of active components in Danqi tablets by HPLC

作　　者：乐世俊 王文晓 高欢 任继国 付瑞嘉 李佳佳 陈艳琰 唐于平 YUE Shi-jun;WANG Wen-Xiao;GAO Huan;REN Ji-guo;FU Rui-jia;LI Jia-jia;CHEN Yan-yan;TANG Yu-ping(Key Laboratory of Shaanxi Administration of Tradotional Chinese Medicine for TCM Compacibility,Shaanxi University of Chinese Medicine,Xi’an 712046,China)

机构地区：[1]陕西中医药大学陕西省中医药管理局中药配伍重点研究室,西安712046

出　　处：《药物分析杂志》2020年第12期2236-2243,共8页Chinese Journal of Pharmaceutical Analysis

基　　金：国家自然科学基金青年基金项目(81903786);陕西省自然科学基金项目(2019JQ-054)。

摘　　要：目的:建立高效液相色谱法同时测定不同厂家丹七片中8个成分的含量。采用聚类分析及主成分分析(PCA)分析法不同厂家丹七片8个成分的规律。方法:采用Waters Sun Fire C18色谱柱(4.6 mm×150 mm,5μm);以乙腈(A)-0.2%磷酸水(B)为流动相,梯度洗脱;流速1.0 mL·min-1;检测波长280 nm(丹参素钠、原儿茶醛、丹酚酸B、丹酚酸A)、203 nm(三七皂苷R1、人参皂苷Rg1、人参皂苷Rb1、人参皂苷Rd);柱温30℃;进样量20μL。结果:4个厂家丹七片样品中8个成分的色谱峰均达到基线分离,丹参素钠、原儿茶醛、丹酚酸B、丹酚酸A、三七皂苷R1、人参皂苷Rg1、人参皂苷Rb1、人参皂苷Rd的线性方程分别为Y=11 347X+2 427.0(r=0.999 9)、Y=98 543X-12 115(r=0.999 9)、Y=25 646X-33 713(r=0.999 8)、Y=52 939X-20 994(r=0.999 8)、Y=5 762.2X+22 415(r=0.999 8)、Y=6 499.1X-21 888(r=0.999 9)、Y=4 877.5X-617.80(r=0.999 9)、Y=6 039.5X-2 993.0(r=0.999 9);平均加样回收率分别为98.3%(RSD=1.9%)、102.3%(RSD=1.3%)、100.2%(RSD=0.47%)、99.1%(RSD=1.1%)、99.1%(RSD=0.88%)、99.2%(RSD=0.86%)、 99.9%(RSD=0.19%)、97.5%(RSD=2.6%);4个厂家丹七片中8个成分的含量分别为丹参素钠1.56~3.23 mg·g^-1、原儿茶醛0.14~0.40 mg·g^-1、丹酚酸B 1.10~7.86 mg·g^-1、丹酚酸A 0.37~1.56 mg·g^-1、三七皂苷R1 4.79~13.12 mg·g^-1、人参皂苷Rg1 26.21~59.10 mg·g^-1、人参皂苷Rb1 17.61~37.05 mg·g^-1、人参皂苷Rd 3.80~8.50 mg·g^-1。基于聚类分析与PCA分析了4个不同厂家不同批次丹七片成分,不同厂家丹七片质量不均一;结论:建立的丹七片中8个成分含量测定方法准确灵敏,稳定性和重复性好,为丹七片的质量研究提供参考。Objective:To establish an HPLC method for simultaneous determination of 8 components in Danqi tablets from four different manufacturers.Cluster analysis and principal component analysis (PCA) were used to analyze the rules of 8 components of Danqi tablets from different manufacturers.Methods:Waters Sun Fire C18 column (4.6 mm×150 mm,5μm) was used with acetonitrile (A)-0.2%phosphate water(B) as mobile phase.The flow rate was 1.0 mL·min-1,the detection wavelength were 280 nm (danshensu sodium,protocatechualdehyde,salvianolic acid B and salvianolic acid A) and 203 nm (notoginsenoside R1,ginsenoside Rg1,ginsenoside Rb1 and ginsenoside Rd),the column temperature was 30℃and the injection volume was 20μL.Results:The chromatographic peaks of 8 components in Danqi tablets from four manufacturers all reached the baseline separation.The linear equations of danshensu sodium,protocatechuic aldehyde,salvianolic acid B,salvianolic acid A,notoginsenoside R1,ginsenoside Rg1,ginsenoside Rb1 and ginsenoside Rd were Y=11 347X+2 427.0 (r=0.999 9),Y=98 543X-12 115 (r=0.999 9),Y=25 646X-33 713(r=0.999 8),Y=52 939X-20 994 (r=0.999 8),Y=5 762.2X+22 415 (r=0.999 8),Y=6 499.1X-21 888 (r=0.999 9),Y=4 877.5X-617.80 (r=0.999 9) and Y=6 039.5X-2 993.0 (r=0.999 9),respectively.The average recovery rates were 98.3%(RSD=1.9%),102.3%(RSD=1.3%),100.2%(RSD=0.47%),99.1%(RSD=1.1%),99.1%(RSD=0.88%),99.2%(RSD=0.86%),99.9%(RSD=0.19%) and 97.5%(RSD=2.6%),respectively.The contents of danshensu sodium,protocatechualdehyde,salvianolic acid B,salvianolic acid A,notoginsenoside R1,ginsenoside Rg1,ginsenoside Rb1 and ginsenoside Rd in Danqi tablets from four manufacturers were 1.56-3.23 mg·g^-1,0.14-0.40 mg·g^-1,1.10-7.86 mg·g^-1,0.37-1.56 mg·g^-1,4.79-13.12 mg·g^-1,26.21-59.10mg·g^-1,17.61-37.05 mg·g^-1 and 3.80-8.50 mg·g^-1,respectively.The components of different batches of Danqi tablets from four different manufacturers were analyzed based on cluster analysis and PCA.The quality of Danqi tablets from the same manufacturer was uniform,but the q

关 键 词：丹七片 高效液相色谱法 含量测定 聚类分析 主成分分析 

分 类 号：R917[医药卫生—药物分析学]