机构地区:[1]联勤保障部队第908医院,江西南昌330002
出 处:《解放军药学学报》2025年第1期43-47,共5页Pharmaceutical Journal of Chinese People's Liberation Army
基 金:江西省中医药管理局科技计划,No.2023B1360。
摘 要:目的建立高效液相色谱波长切换法测定七叶一枝花酊中盐酸表小檗碱,盐酸黄连碱,盐酸巴马汀,盐酸小檗碱,重楼皂苷Ⅰ、Ⅱ、Ⅶ的含量。方法色谱柱为Dimensions C 18柱(4.6 mm×150 mm,5μm),流动相为0.1%磷酸溶液(含4 mg·ml^(-1)庚烷磺酸钠)-乙腈(梯度洗脱),流速为1.0 ml·min-1,检测器为二极管阵列检测器,检测波长分别为0~20 min时345 nm(盐酸表小檗碱、盐酸黄连碱、盐酸巴马汀、盐酸小檗碱)、20~50 min时203 nm(重楼皂苷Ⅰ、Ⅱ、Ⅶ),柱温为室温,进样量为10μl。结果盐酸表小檗碱,盐酸黄连碱,盐酸巴马汀,盐酸小檗碱,重楼皂苷Ⅰ、Ⅱ、Ⅶ分别在21.407~342.512、8.626~138.016、7.080~113.280、6.362~101.792、2.554~40.864、1.921~30.736、1.914~30.624μg·ml^(-1)范围内与峰面积线性关系良好(r≥0.9996,n=6);精密度试验结果的RSD小于2.83%;稳定性试验结果的RSD小于4.63%;重复性试验结果的RSD小于2.96%;加样回收率平均值分别为101.51%、100.75%、98.98%、98.96%、99.41%、99.15%、101.79%,RSD分别为1.44%、2.27%、1.17%、1.49%、2.11%、1.46%、1.54%(n=6)。每毫升七叶一枝花酊分别含盐酸表小檗碱,盐酸黄连碱,盐酸巴马汀,盐酸小檗碱,重楼皂苷Ⅰ、Ⅱ、Ⅶ1.7052,0.6847,0.5644,0.5094,0.2095,0.1548,0.1463 mg(n=3)。结论本研究建立的方法经过方法学验证,可用于七叶一枝花酊中多种成分含量的同时测定。Objective To establish a high performance liquid chromatography with wavelength switching method for the determination of epiberberine hydrochloride,coptisine hydrochloride,palmatine hydrochloride,berberine hydrochloride,Paris Polyphylla saponinⅠ,Paris Polyphylla saponinⅡand Paris Polyphylla saponinⅦin Paris Polyphylla tincture.Methods The samples were separated on Dimensions C 18 column(4.6 mm×150 mm,5μm).The mobile phase consisted of 0.1%phosphoric acid solution(containing 4 mg·ml^(-1) sodium heptanesulfonate)-acetonitrile with gradient elution.The flow rate was 1.0 ml·min-1.The detection wavelengthes was diode array detector(DAD).The detection wavelengths were 345 nm for epiberberine hydrochloride,coptisine hydrochloride,palmatine hydrochloride and berberine hydrochloride at 0-20 min,and 203 nm for Paris Polyphylla saponinⅠ,Paris Polyphylla saponinⅡand Paris Polyphylla saponinⅦat 20-50 min.The column temperature was set at room temperature and the injection volume was 10μl.Results The linear ranges of epiberberine hydrochloride,coptisine hydrochloride,palmatine hydrochloride,berberine hydrochloride,Paris Polyphylla saponinⅠ,Paris Polyphylla saponinⅡand Paris Polyphylla saponinⅦwere 21.407-342.512μg·ml^(-1),8.626-138.016μg·ml^(-1),7.080-113.280μg·ml^(-1),6.362-101.792μg·ml^(-1),2.554-40.864μg·ml^(-1),1.921-30.736μg·ml^(-1),and 1.914-30.624μg·ml^(-1)(r≥0.9996,n=6),respectively.The RSDs of precision tests results were all lower than 2.83%.The RSDs of stability tests results were all lower than 4.63%.The RSDs of repeatability tests results were all lower than 2.96%.The average recoveries of the seven components were 101.51%,100.75%,98.98%,98.96%,99.41%,99.15%and 101.79%with RSDs of 1.44%,2.27%,1.17%,1.49%,2.11%,1.46%and 1.54%(n=6),respectively.The contents of epiberberine hydrochloride,coptisine hydrochloride,palmatine hydrochloride,berberine hydrochloride,Paris Polyphylla saponinⅠ,Paris Polyphylla saponinⅡand Paris Polyphylla saponinⅦin each milliliter Paris Polyphylla
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