HPLC测定黄柏石膏散中盐酸巴马丁和盐酸小檗碱含量

Determination of palmatine hydrochloride and berberine hydrochloride in phellodendron and gypsum powder by HPLC

目的 建立测定黄柏石膏散中盐酸巴马丁和盐酸小檗碱含量的高效液相色谱法。方法 色谱柱:MZ C18柱(4.6 mm×250 mm,5 μm);流动相:水-乙腈(71:29),含0.5％三乙胺、磷酸调pf至3.0;检测波长343 nm;流速:1 mL·min-1。结果 盐酸巴马丁和盐酸小檗碱的理论板数分别为6 500和7 500。盐酸巴马丁回归方程为Y=-433 601+93 680 500X,r=0.999 9,线性范围0.167 4-0.837 2 μg,平均回收率为98.7％(n=5,RSD 1.3％)。盐酸小檗碱回归方程为Y=-887 699+95 231 971X,r=0.999 9,线性范围0.378 9-1.894 μg,平均回收率为99.2％(n=5,RSD 1.6％)。结论 该法操作简便,结果准确,可用于黄柏石膏散中盐酸巴马丁和盐酸小檗碱含量测定。

OBJECTIVE: To develop a quantitative method for the determination of palmatine hydrochloride (PH) and berberine hydrochloride (BH) in phellodendron and gypsum powder by HPLC. METHODS: PH and BH were separated on a MZ C 18 column (4.6 mm × 250 mm, 5 μmn) using a mixture of water and acetonitrile (71:29) as the mobile plase, which was adjusted to pH 3.0 by 0.5% triethylamine solution and phosphoric acid. The flow rate was 1 mL&middotmin-1. The detection wavelength was at 343 nm. RESULTS: The numbers of theoretical plates calculated by PH and BH peak were 6 500 and 7 500 respectively. The regression equation of PH was Y = -433 601 + 93 680 500 X, r = 0.999 9, which was linear over the range of 0.167 4 ∼ 0.837 2 μg. The average recovery was 98.7% (n = 5, RSD 1.3%). The regression equation of BH was Y = 95 231 971 X - 887 699, r = 0.999 9, which was linear over the range of 0.378 9 ∼ 1.894 μg. The average recovery was 99.2% (n = 5, RSD 1.6%). CONCLUSION: The method was sensitive, rapid and accurate.