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作 者:李敏[1,2] 史高峰[1] 柳军玺[2] 邸多隆[2] 刘言娟[2] 冯艳[1,2]
机构地区:[1]兰州理工大学石油化工学院,兰州730050 [2]中国科学院兰州化学物理研究所中国科学院西北特色植物资源化学重点实验室甘肃省天然药物研究重点实验室,兰州730000
出 处:《药物分析杂志》2013年第10期1748-1751,共4页Chinese Journal of Pharmaceutical Analysis
基 金:中科院“西部之光联合学者”、院地合作“全国科学院联盟”项目;甘肃省科技支撑计划(090NKCA127)资助
摘 要:目的:建立异紫堇碱HPLC含量测定和有关物质检查方法。方法:采用SinoChrom ODS-BP C18柱(4.6 mm×250 mm,5μm),以乙腈-三乙胺调至pH 6.02的0.2%磷酸水溶液(50∶50)为流动相,检测波长为270 nm,流速为1.0 mL·min-1,柱温30℃。结果:异紫堇碱与其相关物质峰完全分离,在30~300μg·mL-1浓度范围内呈良好线性关系(n=6),相关系数r=0.9999,定量限为0.03 ng,最低检测限为0.0075 ng,平均回收率99.4%,RSD=2.9%(n=5)。结论:该方法可准确地进行定性、定量检测且专属性好,精密度、准确度符合要求,方法可靠,可用于异紫堇碱的含量及其相关物质的测定。Objective: To develop an HPLC method for the content determination of isocroydine and its related substances. Methods: The determination was performed on a SinoChrom ODS-BP column (4.6 mm × 250 mm,5 μm) with acetonitrile-0.2% (v/v) phosphoric acid in water adjusted by triethylamine to pH 6.02 (50:50) as mobile phase. The flow rate was 1.0 mL·min-1,the detection was set at 270 nm and the column temperature was maintained at 30℃. Results: Isocorydine and its related substances were completely separated. The calibration curve linear between peak and isocorydine concentration was achieved in the range of 30-300 μg·mL-1 (r=0.9999). The limit of detection (LOD) was 0.0075 ng and the limit of quantity (LOQ) was 0.03 ng. The average recovery was 99.4% with RSD 2.9% (n=5). Conclusion: The established method is proved to be specific,accurate and reliable,which can be applied in the determination of isocorydine and its related substances.
关 键 词:异紫堇碱 秃疮花 生物碱含量测定 有关物质 反相高效液相色谱
分 类 号:R917[医药卫生—药物分析学]
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