目的 建立HPLC法同時(shí)測(cè)定癃清片中表小檗堿、黃連堿、鹽酸藥根堿、鹽酸巴馬汀、鹽酸小檗堿、丹皮酚6種成分。方法 Waters SymmetryShield RP18色譜柱(250 mm×4.6 mm,5 μm);流動(dòng)相為乙腈(0.3%甲酸和0.3%三乙胺)-水(0.3%甲酸和0.3%三乙胺),梯度洗脫;體積流量1.0 mL/min;檢測(cè)波長270 nm;柱溫25 ℃;進(jìn)樣體積20 μL。結(jié)果 表小檗堿、黃連堿、鹽酸藥根堿、鹽酸巴馬汀、鹽酸小檗堿、丹皮酚分別在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線性良好,r值均大于0.999 0。平均回收率分別為98.66%、99.49%、99.59%、98.66%、100.40%、99.95%,RSD值分別為2.91%、2.67%、2.65%、1.91%、3.42%、2.28%(n=9)。結(jié)論 該方法專屬性強(qiáng),靈敏度高、重復(fù)性好、簡(jiǎn)單易行,可用于同時(shí)測(cè)定癃清片中表小檗堿、黃連堿、鹽酸藥根堿、鹽酸巴馬汀、鹽酸小檗堿、丹皮酚6種成分,對(duì)完善癃清片的質(zhì)量控制具有參考價(jià)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.