RP-HPLC法测定黄连上清片中盐酸小檗碱、盐酸药根碱和盐酸巴马汀的含量

摘要

OBJECTIVE: To establish the method for the content determination of berberine hydrochloride, jatrorrhizine hydrochloride and palmatine hydrochloride in Huanglian shangqing tablets.METHODS: RP-HPLC method was adopted.The determination was performed on Agilent C18 column with mobile phase consisted of acetonitrile-25 mmoL· L- 1 sodium heptanesulfonate-50 mmoL·L-1 monopotassium phosphate (including 0.14％ triethylamine, pH value adjusted to 3.0 by phosphoric acid, 30∶ 70) at a flow rate of 1.0 mL·min-1.The determination wavelength was set at 348 nm and column temperature was 30 ℃.The injection volume was 5 μL.RESULTS: The linear range of berberine hydrochloride was 40.48～141.70 μg· mL-1 with average recovery of 100.34％ (RSD=1.14％).The linear range of jatrorrhizine hydrochloride was 6.04～14.08 μg· mL-1 with average recovery of 99.70％ (RSD=1.02％).The linear range of palmatine hydrochloride was 10.10～30.30 μg·mL-1 with average recovery of 100.02％ (RSD=l.17％).The contents of berberine hydrochloride, jatrorrhizine hydrochloride and palmatine hydrochloride in three batches of samples were 40.64, 6.09, 10.50; 40.35, 6.05, 10.43; 40.26, 6.03, 10.40 μg per tablet respectively.CONCLUSION: The method is sensitive, accurate, specific and reproducible for content determination of berberine hydrochloride, jatrorrhizinc hydrochloride and palmatine hydrochloride in Huanglian shangqing tablet.%目的:建立测定黄连上清片中盐酸小檗碱、盐酸药根碱和盐酸巴马汀含量的方法.方法:采用反相高效液相色谱法.色谱柱为Agilent C反相柱,流动相为乙腈-25mmoL·L庚烷磺酸钠和50 mmoL·L磷酸二氢钾溶液(含0.14%三乙胺,磷酸调pH至3.0)=30:70,检测波长为348 nm,柱温为30℃,流速为1.0 mL·min,进样量为5 μL.结果:盐酸小檗碱检测浓度在40.48～141.70 μg·mL范围内与峰面积积分值呈良好线性关系,平均加样回收率为100.34%,RSD=1.14%;盐酸药根碱检测浓度在6.04～14.08 μg·mL范围内与峰面积积分值呈良好线性关系,平均加样回收率为99.70%,RSD=1.02%;盐酸巴马汀检测浓度在10.10～30.30 μg·mL范围内与峰面积积分值呈良好线性关系,平均加样回收率为100.02%,RSD=1.17%.3批样品中盐酸小檗碱、盐酸药根碱和盐酸巴马汀的含量分别为每片40.64、6.09、10.50 μg,40.35、6.05、10.43 μg,40.26、6.03、10.40 μg.结论:本方法灵敏、准确,专属性强,重复性好,可作为黄连上清片的质量控制方法.