蛇胆川贝液和蛇胆汁中牛磺胆酸的SPE-HPLC法测定  

Determination of taurocholic acid in Shedanchuanbei Oral Liquid and snake bile by SPE-HPLC

作　　者：朱炳辉[1] 方继辉[2] 李瑾翡[1] 陈焕光[2] 陆惠文[1] 

机构地区：[1]广东省药品检验所,广东广州510180 [2]中山大学化学系,广东广州510275

出　　处：《中成药》2003年第4期281-284,共4页Chinese Traditional Patent Medicine

摘　　要：目的 :建立蛇胆川贝液和蛇胆汁中牛磺胆酸含量的测定方法。方法 :含磷酸二氢钾的样品与甲醇的混合溶液流过Sep PakC18固相萃取微柱。固相萃取微柱吸附溶液中强保留物质以保护分析柱 ,牛磺胆酸被固相萃取微柱饱和吸附后的流出液作反相高效液相色谱法测定用的供试液。色谱条件 :SupelcosilLC 8色谱柱 (15 0mm× 4 .6nm ,5 μm)为分析柱 ,甲醇 0 .4 %磷酸二氢钾溶液 (5 6∶4 4 ,V/V)为流动相 ,检测波长 2 0 3nm ,进样体积为 5 0 μL。 结果 :在 0 .0 2 5 3～0 .2 5 3mg·mL-1浓度范围内 ,牛磺胆酸钠进样浓度与峰面积响应值呈良好的线性关系 ,r =0 .9999;平均回收率为10 1.3% ,RSD为 0 .4 0 % (n =6 )。结论 :本法简便实用 ,分析结果准确可靠 。Objective: To establish the method for determination of taurocholic acid in the Traditional Chinese Medicine Shedanchuanbei Oral Liquid and snake bile. Methods: The sample was prepared as mixed solution containing methanol and KH 2PO 4. The mixed solution was injected into Sep Pak C 18 cartridge for the purpose of sample purity. In this processing, the substances which having strong retain action and could harm analytic column were hold in the Sep Pak C 18 cartridge. The eluting solution that the Sep Pak C 18 cartridge had be over loading for taurocholic acid was used as the test solution. The test solution was measured by RP HPLC. The chromatographic conditions were as followed: Supelcosil LC 8 column(150mm×4.6nm,5μm) as analytic column, detect wavelength at 203nm, and MeOH 0.4%KH 2PO 4 mixed solution(56∶44, V/V ) as mobile phase. The inject volume was 50μL. Results: The linear response range of sodium taurocholate was from 0.0253mg·mL -1 to 0.253mg·mL -1 , and the correlation coefficient was 0.9999. The average recovery rate was 101.3%, RSD was 0.40%( n =6). Conclusion: This method was simple, efficient and suitable to the quality control for Shedanchuanbei Oral Liquid and snake bile.

关 键 词：蛇胆川贝液 蛇胆汁 牛磺胆酸 高效液相色谱法 固相萃取 

分 类 号：R927.2[医药卫生—药学]