HPLC-QAMS同时检测瘀血痹胶囊中10种成分含量  

Simultaneous Determination of 10 Components in Yuxuebi Capsules by HPLC-QAMS

作　　者：曹杰[1] 李阳 任强[2] 周金辉[2] 任红[1] Cao Jie;Li Yang;Ren Qiang;Zhou Jinhui;Ren Hong(Department of Pharmacy,Qingdao Municipal Hospital,Shandong Qingdao 266071,China;College of Pharmacy,Jining Medical University)

机构地区：[1]青岛市市立医院药学部,山东青岛266071 [2]济宁医学院药学院

出　　处：《中国药师》2022年第2期355-359,368,共6页China Pharmacist

基　　金：山东省中医药科技发展计划项目(编号:2019-0449)。

摘　　要：目的:建立高效液相一测多评法(HPLC-QAMS)同步检测瘀血痹胶囊中迷迭香酸、紫草酸、丹酚酸B、羟基红花黄色素A、红花黄色素A、11-羰基-β-乳香酸、11-羰基-β-乙酰乳香酸、α-乳香酸、β-乳香酸和3-乙酰基-β-乳香酸含量的方法。方法:运用Comatex C_(18)色谱柱(250 mm×4.6 mm,5μm),流动相乙腈-0.1%磷酸,梯度洗脱。多波长切换检测(0~24 min检测波长为280 nm,检测迷迭香酸、紫草酸和丹酚酸B,24~34 min检测波长为403 nm,检测羟基红花黄色素A、红花黄色素A,34~65 min检测波长为210 nm,检测11-羰基-β-乳香酸、11-羰基-β-乙酰乳香酸、α-乳香酸、β-乳香酸和3-乙酰基-β-乳香酸)。以11-羰基-β-乙酰乳香酸为内参物,建立其他9种成分的相对校正因子(RCF),并计算各成分含量。采用外标法(ESM)测定瘀血痹胶囊中10种成分含量对一测多评法计算结果的准确性进行验证。结果:测定了12批瘀血痹胶囊中上述成分的含量,10种成分分别在0.99~49.50μg·ml^(-1),1.16~58.00μg·ml^(-1),17.58~879.00μg·ml^(-1),2.39~119.50μg·ml^(-1),1.36~68.00μg·ml^(-1),3.65~182.50μg·ml^(-1),9.28~464.00μg·ml^(-1),1.77~88.50μg·ml^(-1),4.09~204.50μg·ml^(-1),4.78~239.00μg·ml^(-1)(r=0.9994)范围内有良好的线性关系。平均加样回收率及RSD分别为96.95%(1.08%),98.30%(1.33%),100.03%(0.82%),98.84%(0.76%),97.12%(1.27%),99.50%(1.10%),100.09%(0.65%),98.05%(1.50%),97.79%(1.17%),99.23%(0.96%)(n=9)。一测多评法所测结果与外标法差异无统计学意义。结论:该方法可用于瘀血痹胶囊中10种成分含量的同步测定,达到多指标质量控制的目的。Objective:To establish a method of high performance liquid chromatography with quantitative analysis of multi-components by single marker(HPLC-QAMS)to simultaneously determine the contents of rosmarinic acid,lithospermic acid,salvianolic acid B,hydroxysafflor yellow A,safflor yellow A,11-keto-β-boswellic acid,3-acetyl-11-keto-β-boswellic acid,α-boswellic acid,β-boswellic acid and 3-acetyl-β-boswellic acid in Yuxuebi capsules.Methods:The separation was carried out on a Comatex C_(18)column(250 mm×4.6 mm,5μm).The mobile phase consisted of acetonitrile-0.1%phosphoric acid with gradient elution.The detection wavelengths were with multi-wavelength switching(0-24 min,280 nm for rosmarinic acid,lithospermic acid and salvianolic acid B;24-34 min,403 nm for hydroxysafflor yellow A and safflor yellow A;34-65 min,210 nm for 11-keto-β-boswellic acid,3-acetyl-11-keto-β-boswellic acid,α-boswellic acid,β-boswellic acid and 3-acetyl-β-boswellic acid).Using 3-acetyl-11-keto-β-boswellic acid as the internal standard,the relative correction factor(RCF)of the other nine components was established and the contents of each component were calculated.In order to validate the accuracy,the ten components in Yuxuebi capsules were determined and compared by both HPLC-QAMS and an external standard method(ESM).Results:The contents of ten components in 12 batches of Yuxuebi capsules were determined,and they showed good linear relationships within the ranges of 0.99-49.50μg·ml^(-1),1.16-58.00μg·ml^(-1),17.58-879.00μg·ml^(-1),2.39-119.50μg·ml^(-1),1.36-68.00μg·ml^(-1),3.65-182.50μg·ml^(-1),9.28-464.00μg·ml^(-1),1.77-88.50μg·ml^(-1),4.09-204.50μg·ml^(-1)and 4.78-239.00μg·ml^(-1)(r≥0.9994),and the average recoveries(RSDs)were 96.95%(1.08%),98.30%(1.33%),100.03%(0.82%),98.84%(0.76%),97.12%(1.27%),99.50%(1.10%),100.09%(0.65%),98.05%(1.50%),97.79%(1.17%)and 99.23%(0.96%)(n=9),respectively.The differences between HPLC-QAMS and ESM had no statistical significance.Conclusion:The method can be used for the simultaneous

关 键 词：瘀血痹胶囊 高效液相一测多评法 多指标成分 相对校正因子 

分 类 号：R927.2[医药卫生—药学]