SPE-HPLC测定乐舒洗液中黄柏碱含量

摘要

目的 建立乐舒洗液中黄柏的薄层鉴别,以及用固相萃取-高效液相色谱法(SPE-HPLC)测定黄柏碱含量的方法.方法 采用薄层色谱法对乐舒洗液中的黄柏进行定性鉴别.采用Bond Elut plexa PCX强阳离子交换固相萃取小柱净化,Platisil-NH2柱为色谱柱,柱温为30℃,流动相为0.3%三乙胺(磷酸调pH 3.82)-四氢呋喃-乙腈(18:12:70),等度洗脱,流速为1.0 mL/min,检测波长为286 nm,测定乐舒洗液中黄柏碱的含量.结果 薄层色谱法能明显检出黄柏的特征有效成分黄柏碱;黄柏碱在1.22~12.2μg(r=0.9999)范围内与峰面积线性关系良好,平均加样回收率为101.18%,RSD=1.71%.结论 本方法操作简单,准确性、重复性好,可用于乐舒洗液的质量控制.%Objective To establish the method of thin layer identification of Phellodendri Chinensis Cortex and solid phase extraction - high performance liquid chromatography (SPE-HPLC) determination of the content of phellodendrine in Leshu Lotion. Methods Thin layer chromatography (TLC) was used for qualitative identification of Phellodendri Chinensis Cortex in Leshu Lotion and the Bond Elutplexa PCX strong cation-exchange solid phase was used for extraction small column purification. Platisil-NH2 column was as chromatographic column; column temperature was 30 ℃; triethylamine pH 3.82 (phosphoric acid), tetrahydrofuran, acetonitrile was 18:12:70, isocratic elution; flow rate was 1.0 mL/min; detection wavelength was 286 nm. Results TLC could obviously identify active ingredients of phellodendrine in Phellodendri Chinensis Cortex. The phellodendrine had good linear relationship between concentration and peak area within the scope of 1.22–12.2 μg (r=0.9999); the average recovery rate of phellodendrine was 101.18%, RSD was 1.71%. Conclusion This method is simple to operate, with accuracy and repeatability, and can be used for quality control of Leshu Lotion.