首页|HPLC法同时测定复方双花片中10个成分的含量

HPLC法同时测定复方双花片中10个成分的含量

扫码查看
目的:采用高效液相色谱(HPLC)技术,建立同时测定复方双花片中新绿原酸、绿原酸、隐绿原酸、连翘酯苷A、3,4-二-O-咖啡酰奎宁酸、3,5-二-O-咖啡酰奎宁酸、4,5-二-O-咖啡酰奎宁酸、连翘苷、穿心莲内酯和脱水穿心莲内酯10个成分含量的方法.方法:复方双花片样品用50%甲醇水超声提取,采用Agilent Zorbax SB-C18(250 mm ×4.6 mm,5μm)色谱柱分析,流动相为乙腈-0.15%磷酸水溶液,梯度洗脱,流速1.0 mL·min-1,柱温30 ℃,进样量10 μL,检测波长327 nm(检测新绿原酸、绿原酸、隐绿原酸、连翘酯苷A、3,4-二-O-咖啡酰奎宁酸、3,5-二-O-咖啡酰奎宁酸、4,5-二-O-咖啡酰奎宁酸)和226 nm(检测连翘苷、穿心莲内酯、脱水穿心莲内酯).结果:新绿原酸、绿原酸、隐绿原酸、连翘酯苷A、3,4-二-O-咖啡酰奎宁酸、3,5-二-O-咖啡酰奎宁酸、4,5-二-O-咖啡酰奎宁酸、连翘苷、穿心莲内酯和脱水穿心莲内酯质量浓度分别在 4.071~40.71 μg·mL-1(r=0.999 9)、20.16~201.6 μg·mL 1(r=0.999 9)、4.730~47.30 μg·mL-1(r=0.999 9)、4.536~45.36μg·mL-1(r=0.999 8)、1.817~18.17μg·mL-1(r=0.999 9)、2.266~22.66 μg·mL-1(r=0.999 7)、3.321~33.21 μg·mL-1(r=0.999 9)、3.462~34.62 μg·mL-1(r=0.999 6)、2.111~21.11 μg·mL-1(r=0.999 9)和 2.290~22.90μg·mL-1(r=0.999 7)与峰面积呈良好的线性关系;平均回收率(RSD)(n=6)分别为101.3%(2.1%)、103.0%(1.5%)、100.9%(2.0%)、101.1%(2.0%)、98.4%(1.6%)、102.2%(2.4%)、98.2%(1.3%)、97.8%(2.0%)、99.0%(2.0%)和96.4%(1.1%);4 批样品中上述 10 个成分的含量分别为 1.685~2.649 mg·g 12.202~13.780 mg·g-1、2.415~2.594 mg·g-1、1.340~1.919 mg·g-1、0.501~0.791 mg·g-1、0.891~1.342 mg·g-1、1.299~2.105 mg·g-1、1.147~1.504 mg·g-1、0.654~0.694 mg·g 10.846~1.151 mg·g-1.结论:所建立的方法简单准确,可用于复方双花片的质量控制与评价.
Simultaneous determination of ten constituents in compound Shuanghua tablets by HPLC
Objective:To establish an HPLC method for simultaneous determination of neochlorogenic acid,chlorogenic acid,cryptochlorogenic acid,forsythiaside A,3,4-O-dicaffeoylquinic acid,3,5-O-dicaf-feoylquinic acid,4,5-O-dicaffeoylquinic acid,forsythin,andrographalide and dehydroandrographalide in com-pound Shuanghua tablets.Methods:The samples were extracted with 50%methanol solution under ultrasonic condition,and were performed on Agilent Zoabax SB-C18 column(250 mm ×4.6 mm,5 μm)by gradient elution of acetonitrile-0.15%phosphoric acid solution at a flow rate of 1.0 mL·min-1.The column temperature was 30 ℃,the injection volume was 10 μL,and the detection wavelength were set at 327 nm(detecting neochlorogenic acid,chlorogenic acid,cryptochlorogenic acid,forsythiaside A,3,4-O-dicaffeoylquinic acid,3,5-O-dicaf-feoylquinic acid and 4,5-O-dicaffeoylquinic acid)and 226 nm(detecting forsythin,andrographalide and dehydroandrographalide).Results:The linear ranges of neochlorogenic acid,chlorogenic acid,cryptochlorogenic acid,forsythiaside A,3,4-O-dicaffeoylquinic acid,3,5-O-dicaffeoylquinic acid,4,5-O-dicaffeoylquinic acid,forsythin,andrographalide and dehydroandrographalide were 4.071-40.71 μg·mL-1(r=0.999 9),20.16-201.6 μg·mL-1(r=0.999 9),4.730-47.30 μg·mL-1(r=0.999 9),4.536-45.36 μg·mL-1(r=0.999 8),1.817-18.17 μg·mL-1(r=0.999 9),2.266-22.66 μg·mL-1(r=0.999 7),3.321-33.21μg·mL-1(r=0.999 9),3.462-34.62 μg·mL-1(r=0.999 6),2.111-21.11 μg·mL-1(r=0.999 9)and 2.290-22.90 μg·mL-1(r=0.999 7),respectively.The average recoveries(n=6)were 101.3%(2.1%),103.0%(1.5%),100.9%(2.0%),101.1%(2.0%),98.4%(1.6%),102.2%(2.4%),98.2%(1.3%),97.8%(2.0%),99.0%(2.0%)and 96.4%(1.1%),respectively.The contents of the 10 components in 4 bacthes of Fufang Shuanghua tablets were in the range of 1.685-2.649 mg·g-1,12.202-13.780 mg·g-1,2.415-2.594 mg·g-1,1.340-1.919 mg·g-1,0.501-0.791 mg·g-1,0.891-1.342 mg·g-1,1.299-2.105 mg·g-1,1.147-1.504 mg·g-1,0.654-0.694 mg·g-1,0.846-1.151 mg·g-1,respectively.Conclusion:This simple accurate reproducible method can be used for the quality control and evaluate of compound Shuanghua tablets.

compound Shuanghua tabletsHPLCchemical constituentscontent determinationquality control

尚朝利、白泽方、樊轻亚

展开 >

信阳职业技术学院,信阳 464000

复方双花片 高效液相色谱 化学成分 含量测定 质量控制

2024

药物分析杂志
中国药学会

药物分析杂志

CSTPCD北大核心
影响因子:1.039
ISSN:0254-1793
年,卷(期):2024.44(2)
  • 15