目的 建立一种高效液相色谱-电喷雾检测器（HPLC-CAD）法分离测定三金片中积雪草苷B和羟基积雪草苷2个同分异构体含量的方法。方法 采用Thermo Acclaim^TMC₃₀色谱柱，甲醇-乙腈-水（35∶8∶57）为流动相，柱温35 ℃，CAD气化温度为50 ℃，采集频率为10 Hz，分离测定积雪草苷B和羟基积雪草苷的含量。结果 积雪草苷B和羟基积雪草苷线性关系良好，r分别为0.999 8、0.998 4，线性范围分别为0.240 7～2.406 9、0.573 1～5.730 8 μg，平均加样回收率分别为100.26%、98.32%，RSD分别为0.69%、1.78%；11批样品中积雪草苷B为1.65～3.18 mg/g，羟基积雪草苷为3.49～7.90 mg/g。结论 该方法简便、灵敏、准确度高，能有效分离测定积雪草苷B和羟基积雪草苷2个同分异构体，可用于三金片现行药典标准的提高完善。

Objective To establish a HPLC-CAD method for the determination of asiaticoside B and madecassoside in Sanjin Tablets (三金片). Methods The separation was performed on Thermo Acclaim^TMC₃₀ column (250 mm×4.6 mm, 5 mm) with the mobile phase of methanol-acetonitrile-water (35∶8∶57). The flow rate was 1.0 mL/min and the column temperature was 35 ℃. CAD detection condition included that the nebulization temperature was 50 ℃ and data acquisition frequency was 10 Hz. The content of asiaticoside B and madecassoside was determinated. Results The linear ranges of asiaticoside B and madecassoside were 0.240 7—2.406 9 μg (r = 0.999 8) and 0.573 1—5.730 8 μg (r = 0.998 4), respectively. The average recoveries of asiaticoside B and madecassoside were 100.26% (RSD 0.69%) and 98.32% (RSD 1.78%), respectively. The contents of asiaticoside B and madecassoside in 11 batches of samples were 1.65—3.18 mg/g and 3.49—7.90 mg/g. Conclusion The method is accurate, convenient and sensitive for the quality control of two isomers (asiaticoside B and madecassoside) in Sanjin Tablets.

R286.02

广西创新驱动发展科技重大专项（桂科AA17202045）