目的 建立反相-高效液相色谱(RP-HPLC)法测定保肝丸中马钱素、芍药苷和黄芩素的量,为保肝丸应用于对伴有基础肝病肝脏的保护与再生作用的动物实验提供质量保证.方法 采用安捷伦Zorbax SB-C₁₈(150 mm×4.6 mm,5 μm)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 mL/min;紫外检测波长马钱素与芍药苷为236 nm,黄芩素为278 nm;柱温30 ℃;进样量为5 μL.结果 马钱素的最低检测质量浓度为14.3 μg/L,线性范围为7.305～233.750 mg/L,精密度RSD为1.69%;芍药苷的最低检测质量浓度为30.9 μg/L,线性范围为5.742～183.750 mg/L,精密度RSD为1.86%;黄芩素的最低检测质量浓度为36.4 μg/L,线性范围为3.711～118.750 mg/L,精密度RSD为1.76%;保肝丸中马钱素的平均回收率为99.2%,RSD为1.66%;芍药苷的平均回收率为98.9%、RSD为1.82%;黄芩素的平均回收率为100.6%,RSD为1.90%.结论 该方法简便、灵敏度高、重复性好、平均回收率高,是检测马钱素、芍药苷和黄芩素质量浓度的可信方法.

Objective To establish a method of RP-HPLC for determining the mass concentration of loganin, paeoniflorin and baicalein in Baogan Pills, and it has provided the quality guarantee for the animal experiment which applied to the liver protection and reproductive function together with the basis of liver disease. Methods Agilent Zorbax SB-C₁₈ (150 mm × 46 mm, 5 μm) column was used. Acetonitrile and 0.1% phosphoric acid water-solution were used as mobile phase in gradient elution. The volume flow was at 1.0 mL/min; ultraviolent detection wavelength was 236 nm when loganin and paeoniflorin were detected, and was 278 nm when baicalein was detected; Column temperature was at 30 ℃ and injection volume was 5 μL. Results The lowest detection limit in loganin was 14.3 μg/L, the linear range was 7.305—233.750 mg/L, and its RSD was 1.69%; The lowest detection limit in paeoniflorin was 30.9 μg/L, the linear range was 5.742—183.750 mg/L, and its RSD was 1.86%; The lowest detection limit in baicalein was 36.4 μg/L, the linear range was 3.711—118.750 mg/L, and its RSD was 1.76 %. The average recovery of loganin in Baogan Pills was 99.2%, and its RSD was 1.66%; The average recovery of paeoniflorin was 98.9%, and its RSD was 1.82 %; The average recovery of baicalein in was 100.6%, and its RSD was 1.90%. Conclusion The method is believable for determining the mass concentration of loganin, paeoniflorin, and baicalein with its simplicity, sensibility, repeatability, and better recovery rate.

天津市应用基础与前沿技术研究计划(14JCYBJC24800)