HPLC测定附杞固本膏中单酯型生物碱的含量
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云南白药集团创新研发中心/云南省药物研究所/云南省中药和民族药新药创制企业重点实验室,云南 昆明 650111

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R286

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* 基金项目: 云南省科技计划项目(2014DC036) 收稿日期: 2016 - 01 - 18 作者简介: 刘佳(1982-),女,云南昆明人,工程师,研究方向:天然药物化学研究。△通信作者:冯莉萍,E-mail:67501903@qq.com


Content Determination of Monoester Aconitum Alkaloids in Paste of Fuqi Guben by HPLC
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Yunnan Institute of Materia Medica, Kunming 650111, China

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    摘要:

    目的建立附杞固本膏中单酯型生物碱的高效液相色谱含量测定方法。方法色谱柱Waters XTerra RP18 5mm(4.6mm×250mm);柱温30℃;流动相:以乙腈-四氢呋喃(25∶15)为流动相A,以0.1mol/L醋酸铵溶液(每1000mL含冰醋酸0.5mL)为流动相B,进行梯度洗脱;流速1.0mL/min;检测波长为235nm。结果经方法学验证表明,苯甲酰新乌头原碱、苯甲酰乌头原碱和苯甲酰次乌头原碱分别在0.045-1.800μg、0.0425-1.7000μg、0.0442-1.7680μg范围内呈线性关系,精密度、稳定性、重现性均符合要求,本测定方法的平均回收率分别为99.89%、99.22%、101.12%,RSD为1.72%、1.75%、2.32%(n=6)。结论该方法简便、快速、准确、无干扰,可用于该制剂的质量控制。

    Abstract:

    Objective Establishing a HPLC method for the determination of monoester aconitum alkaloids in paste of Fuqi Guben. Methods Column Waters XTerra RP18 5mm(4.6mm×250mm); column temperature was 30℃; Acetonitrile -tetrahydrofuran(25∶15) as the mobile phase A, 0.1mol/L ammonium acetate solution(1000mL containing glacial acetic acid per 0.5mL) as the mobile phase B, gradient elution, flow rate was 1 mL/min, the detection wavelength was 254 nm. Results Benzoylmesaconine is in the range of 0.045~1.800μg showed a linear relationship, benzoylaconitine is in the range of 0.0425~1.7000μg showed a linear relationship, and benzoylhypacoitine is in the range of 0.0442~1.7680μg showed a linear relationship. Precision, stability, reproducibility are in line with the requirements, the average recovery of this measurement method were 99.89%, 99.22%, 101.12%, RSD was 1.72%, 1.75%, 2.32%(n=6). Conclusion The method was so convenient, fast, accurate and no interference that it can be used for quality control of the preparation.

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