目的 建立HPLC法同时测定癃清片中表小檗碱、黄连碱、盐酸药根碱、盐酸巴马汀、盐酸小檗碱、丹皮酚6种成分。方法 Waters SymmetryShield RP18色谱柱(250 mm×4.6 mm,5 μm);流动相为乙腈(0.3%甲酸和0.3%三乙胺)-水(0.3%甲酸和0.3%三乙胺),梯度洗脱;体积流量1.0 mL/min;检测波长270 nm;柱温25 ℃;进样体积20 μL。结果 表小檗碱、黄连碱、盐酸药根碱、盐酸巴马汀、盐酸小檗碱、丹皮酚分别在1.856～18.56、14.230～142.30、1.070～10.79、2.485～24.85、38.915～389.15、9.824～98.24 μg/mL线性良好,r值均大于0.999 0。平均回收率分别为98.66%、99.49%、99.59%、98.66%、100.40%、99.95%,RSD值分别为2.91%、2.67%、2.65%、1.91%、3.42%、2.28%(n=9)。结论 该方法专属性强,灵敏度高、重复性好、简单易行,可用于同时测定癃清片中表小檗碱、黄连碱、盐酸药根碱、盐酸巴马汀、盐酸小檗碱、丹皮酚6种成分,对完善癃清片的质量控制具有参考价值。

Objective To develop an HPLC method for simultaneous determination of epiberberine, coptisine, jatrorrhizin, palmatine, berberine, and paeonol in Longqing Tablets. Methods The analysis was performed on Waters Symmetry Shield TM RP18 column (250 mm × 4.6 mm, 5 μm) with cetonitrile (0.3% triethylamine and 0.3% phosphoric acid) - water (0.3% triethylamine and 0.3% phosphoric acid) as mobile phases for gradient elution. The flow rate was 1.0 mL/min. The detection wavelength was set at 270 nm. The column temperature was 25 ℃ with injection volume of 20 μL. Results Epiberberine, coptisine, jatronhizine, palmatine, berberine, and paeonol had good linearity in the ranges of 1.856 — 18.56, 14.230 — 142.30, 1.070 — 10.79, 2.485 — 24.85, 38.915 — 389.15, and 9.824 — 98.24 μg/mL, respectively. The correlation coefficients of all curves were above 0.999 0. The average recoveries were 98.66%, 99.49%, 99.59%, 98.66%, 100.40%, and 99.95% with RSD 2.91%, 2.67%, 2.65%, 1.91%, 3.42%, and 2.28% (n=9), respectively. Conclusion The method is specific, sensitive, repeatable, and simple for simultancous determinationg of epiberberine, coptisine, jatronhizine, palmatine, berberine and paeonol, which can be available for the quality control of Longqing Tablets.