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 tincture were 1.7052,0.6847,0.5644,0.5094,0.2095,0.1548 and 0.1463 mg(n=3),respectively.Conclusion The established method has been validated,which can be used for simultaneous determination of multiple components of Paris Polyphylla tincture.
作者
肖汉扬
吴骏
李刚
张增珠
谢小洁
邓雯
胡文弋
徐兰
XIAO Han-yang;WU Jun;LI Gang;ZHANG Zeng-zhu;XIE Xiao-jie;DENG Wen;HU Wen-yi;XU Lan(The 908th Hospital of the Joint Logistic Support Force of PLA,Nanchang 330002,China)
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。
关键词
高效液相色谱法
波长切换法
七叶一枝花酊
含量测定
HPLC
switching wavelength method
Paris Polyphylla tincture
content determination
作者简介
肖汉扬,大学本科,主管药师。研究方向:医院制剂。E-mail:328860637@qq.com;通信作者:徐兰,主管药师。E-mail:xulan2005112056@126.com。
