HPLC梯度洗脱-多波长切换法同时测定固肾丸中4种成分含量  

Simultaneous Determination of Four Components in Gushen Pill by HPLC Gradient Elution Multi Wavelength Switching Method

作　　者：李鹂 贺蓓蓓 黄良永 杜士明 LI Li;HE Beibei;HUANG Liangyong;DU Shiming(Department of Pharmacy,Taihe Hospital Affiliated with Hubei University of Medicine,Shiyan 442000,China;Department of Pharmacology,Hubei University of Medicine,Shiyan 442000,China;Hubei Key Laboratory of Wudang Local Chinese Medicine Research(Hubei University of Medicine),Shiyan 442000,China)

机构地区：[1]十堰市太和医院(湖北医药学院附属医院)药学部,十堰442000 [2]湖北医药学院药学院,十堰442000 [3]武当特色中药研究湖北省重点实验室(湖北医药学院),十堰442000

出　　处：《医药导报》2022年第12期1841-1845,共5页Herald of Medicine

基　　金：湖北省卫生健康委中医药科研立项项目(ZY2021M005)。

摘　　要：目的建立同时测定固肾丸中红景天苷、芍药苷、二苯乙烯苷、淫羊藿苷4种成分含量的高效液相色谱(HPLC)方法,为修订该制剂的质量标准提供依据。方法运用HPLC梯度洗脱-多波长切换法。色谱柱:OMNIBond HPLC column Orca C_(18)(250 mm×4.6 mm,5μm),流动相:乙腈-0.1%磷酸溶液(梯度洗脱),流速:1.0 mL·min^(-1),检测波长:220 nm(红景天苷)、230 nm(芍药苷)、320 nm(二苯乙烯苷)、270 nm(淫羊藿苷),柱温:30℃,进样量:10μL。结果4种成分的分离度均良好,阴性对照不产生干扰。红景天苷、芍药苷、二苯乙烯苷、淫羊藿苷浓度分别在2.67~267.35,5.76~575.95,3.60~360.29,4.29~429.20μg·mL^(-1)范围内与其峰面积有良好的线性关系(R^(2)≥0.9997);精密度、重复性和稳定性(24 h)实验的RSD均<2%(n=6);平均加样回收率分别为101.41%,98.47%,101.32%,101.55%,RSD均<2.0%(n=6)。结论该研究所建立的HPLC梯度洗脱-多波长切换法操作简便、专属性强、稳定性好,可用于固肾丸中红景天苷、芍药苷、二苯乙烯苷、淫羊藿苷4种成分含量的同时测定。Objective To establish an HPLC method for simultaneous determination of salidroside,paeoniflorin,2,3,5,4'-tetrahydroxy stilbene-2-O-β-D-glucoside and icariin in Gushen pill,to provide a basis for revising the quality standard of the preparation.Methods The analysis was performed on an OMNIBond Orca C_(18) column(250 mm×4.6 mm,5μm),the mobile phase of acetonitrile-0.1%phosphoric acid aqueous solution in a linear gradient mode.The flow rate was 1.0 mL·min^(-1).The detection wavelengths were set at 220 nm for salidroside,230 nm for paeoniflorin,270 nm for icariin,and 320 nm for 2,3,5,4'-tetrahydroxy stilbene-2-O-β-D-glucoside.The column temperature was 30℃.The injection volume was 10μL.Results The separation of the four components was good,and the negative control did not interfere.Salidroside,paeoniflorin,icariin,and 2,3,5,4'-Tetrahydroxy stilbene-2-O-β-D-glucoside showed good linear relationships within the ranges of 2.67-267.35,5.76-575.95,4.29-429.20 and 3.60-360.29μg·mL^(-1)(R^(2)≥0.9997),respectively.The RSD of precision,repeatability,and stability(24 h)tests were less than 2.0%;The average recoveries were 101.41%,98.47%,101.32%,and 101.55%,respectively,and the RSD was less than 2.0%.Conclusion The HPLC method is simple,accurate,and reproducible,which can be used to simultaneously determine salidroside,paeoniflorin,2,3,5,4'-tetrahydroxy stilbene-2-O-β-D-glucoside and icariin in Gushen pills.

关 键 词：固肾丸 含量测定 高效液相色谱法 多波长切换 

分 类 号：R289.5[医药卫生—方剂学] R917[医药卫生—中药学]