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该研究建立了盐酸去亚甲基小檗碱含量测定的HPLC分析方法。采用Agilent ZORBAX SB-C18(4.6 mm×150 mm,5μm)色谱柱,以50 mmol/L磷酸二氢钾缓冲液(磷酸调节p H值至3.0)为流动相A,乙腈为流动相B,进行梯度洗脱,体积流量1 m L/min;检测波长349 nm;柱温30℃。结果表明,盐酸去亚甲基小檗碱供试品溶液在2~200μg/m L范围内浓度和峰面积成良好的线性关系,相关系数R为0.999 6,日内和日间精密度的RSD(%)均小于2%;平均回收率为101.6%,RSD(%)为1.0%。重复性和稳定性的RSD(%)分别为1.2%和0.8%。3批盐酸去亚甲基小檗碱原料药中盐酸去亚甲基小檗碱含量为97.8%,98.4%,98.2%。HPLC法测定盐酸去亚甲基小檗碱的含量具有较好的专属性和灵敏度,准确度高,且操作简便,重复性好。该方法可用于盐酸去亚甲基小檗碱的含量分析和质量控制。
The study established a method for the determination of desmethylberberry hydrochloride by HPLC. The mobile phase A was acetonitrile (50%), mobile phase B (pH = 3.0 with phosphoric acid), using an Agilent ZORBAX SB-C18 column (4.6 mm × 150 mm, 5 μm) Gradient elution, volume flow 1 m L / min; detection wavelength 349 nm; column temperature 30 ℃. The results showed that there was a good linear relationship between the concentration and the peak area of desmethylated hydrochloric berberine in the range of 2 ~ 200μg / m L, the correlation coefficient R was 0.999 6, RSD (intra-day and inter-day precision) %) Were less than 2%; the average recovery was 101.6% and the RSD (%) was 1.0%. RSD (%) for repeatability and stability were 1.2% and 0.8%, respectively. 3 batches of desmethylene hydrochloride berberine hydrochloride raw material to the content of methylene berberine 97.8%, 98.4%, 98.2%. HPLC method for the determination of the content of methylene blue berberine has good specificity and sensitivity, high accuracy, and easy to operate, good repeatability. The method can be used for content analysis and quality control of demethyl-berberine hydrochloride.