RP-HPLC同时测定护肝剂中9种活性成分  

Simultaneous determination of nine kinds of active components in Hugan Agent by RP-HPLC

作　　者：刘宏胜[1] 王树森[1] 张雅敏[2] 刘子荣[2] 赵晨翔[2] 

机构地区：[1]天津市第一中心医院卫生部危重病急救医学重点实验室,天津300192 [2]天津市第一中心医院肝胆外科,天津300192

出　　处：《中草药》2016年第6期933-937,共5页Chinese Traditional and Herbal Drugs

基　　金：天津市应用基础与前沿技术研究计划(14JCYBJC24800)

摘　　要：目的建立RP-HPLC法同时测定护肝剂中马钱素、芍药苷、野黄芩苷、黄芩苷、黄芩素、五味子甲素、五味子乙素、五味子丙素和熊果酸9种中药活性成分,为护肝剂的制剂质量提供保障。方法采用安捷伦Zorbax SB-C18（150 mm×4.6mm,5μm）色谱柱;流动相为乙腈-0.1%磷酸水溶液,梯度洗脱,体积流量1.0 m L/min;紫外检测波长为236、280、210 nm;柱温30℃;进样量为5μL。结果马钱素、芍药苷、野黄芩苷、黄芩苷、黄芩素、五味子甲素、五味子乙素、五味子丙素和熊果酸的最低检测限分别为12.0、2.60、5.75、9.75、14.39、19.06、14.90、15.63、16.08 ng;线性范围分别为583.33~18.229、916.67~28.65、541.67~16.93、416.67~13.02、500.00~15.63、458.33~14.32、625.00~19.53、458.33~14.32、1 000.00~31.25 mg/L;平均加样回收率分别为103.51%、104.19%、95.16%、96.71%、105.61%、96.12%、97.09%、96.87%、105.90%;精密度RSD分别为1.25%、1.31%、1.91%、1.88%、1.95%、1.45%、1.66%、1.52%、1.33%;重复性RSD分别为1.39%、1.41%、1.87%、1.91%、1.79%、1.45%、1.32%、1.71%、1.49%;稳定性RSD分别为1.36%、1.22%、1.87%、1.91%、1.93%、1.56%、1.39%、1.78%、1.61%。6批护肝剂中含马钱素、熊果酸、芍药苷、野黄芩苷、黄芩苷、黄芩素、五味子甲素、乙素及丙素的平均质量浓度分别在216.5~222.5、40.8~42.8、125.4~136.3、144.0~147.3、1 640.8~1 947.3、497.5~515.0、15.0~17.3、33.6~36.0、3.0~3.9 mg/L。结论该方法简便、灵敏度高、重复性好、平均回收率高,是检测护肝剂中马钱素、芍药苷、野黄芩苷、黄芩苷、黄芩素、五味子甲素、五味子乙素、五味子丙素和熊果酸的可信方法。Objective To establish an RP-HPLC method for simultaneous determining the contents of nine kinds of components in Hugan Agent such as loganin, paeonflorin, scuteuarin, baicalin, baicalein, deoxyschizandrin, schisandrin, schizandrin G, and ursolic acid, and to provide the quality guarantee for it. Methods Agilent Zorbax SB-C18 （150 mm × 4.6 mm, 5 μm） column was used. Acetonitrile and 0.1% phosphoric acid water-solution were used as mobile phase of gradient elution, and the volume flow was at 1.0 mL/min; Ultraviolent determination wavelength was 236, 280, and 210 ran; Column temperature was at 30 ℃, and injection volume was 5 μL. Results The lowest detection limit in loganin, paeonflorin, scuteuarin, baicalin, baicalein, deoxyschizandrin, schisandrin, schizandrin C, and ursotic acid respectively was 12.0, 2.60, 5.75, 9.75, 14.39, 19.06, 14.90, 15.63, and 16.08 ng; The linear range was 583.33-18.229, 9!6.67-28.65,541.67-16.93,416.67-13.02,500.00-15.63,458.33-14.32, 625.00-19.53,458.33-14.32, and 1 000.00-31.25 mg/L, respectively; The average recovery in Hugan Agent was 103.51%, 104.19%, 95.16%, 96.71%, 105.61%, 96.12%, 9%09%, 96.87%, and 105.90%, respectively, The repeatabilit;y RSD was 1.39%,1.41%, 1.87%, 1.91%, 1.79%, 1.45%, 1.32%,1.71%, and 1.49%, respectively; The stability RSD was 1.36%, 1.22%, 1.87%, 1.91%, 1.93%, 1.56%, 1.39%, 1.78%, and 1.61%, respectively. 6 batche of Hugan Agent contained the average quality of loganin, ursolic acid, paeonflorin, scuteuarin, baicalin, baicalein deoxyschizandrin, schisandrin, and schizandrin respectively was 216.5-222.5, 40.8-42.8, 125.4-136.3, 144.0-147.3, 1 640.8-1 947.3, 497.5-515.0, 15.0-17.3, 33.6-36.0, and 3.0-3.9 mg/L. Conclusion The method is believable for determining the concent of loganin, paeonflorin, scuteuarin, baicalin, baicalein, deoxyschizandrin, schisandrin, schizandrin C, and ursolic acid in Hugan Agent with its simplicity, sensibility, repeatability, and better recovery rate.

关 键 词：护肝剂 RP-HPLC 马钱素 芍药苷 野黄芩苷 黄芩苷 黄芩素 五味子甲素 五味子乙素 五味子丙素 熊果酸 山茱萸 黄芩 五味子 白芍 

分 类 号：R286.02[医药卫生—中药学]