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机构地区:[1]江苏省食品药品检验所,南京210008 [2]南京中医药大学,南京210046
出 处:《中药新药与临床药理》2009年第1期41-43,共3页Traditional Chinese Drug Research and Clinical Pharmacology
摘 要:目的建立益气止血颗粒中盐酸小檗碱、盐酸巴马汀和盐酸药根碱的含量测定方法。方法采用甲醇超声提取,反相离子对高效液相色谱法测定。C18柱分离;柱温30℃;流动相为0.01mol/L庚烷磺酸钠与0.01mol/L磷酸二氢钾等量混合溶液(用磷酸调pH=3.1)-乙腈(70∶30);流速1.0mL/min;检测波长为345nm。结果3种生物碱成分色谱分离行为良好,平均回收率(n=6)分别为盐酸小檗碱100.95%,RSD=2.10%;盐酸巴马汀102.14%,RSD=2.29%;盐酸药根碱100.71%,RSD=2.65%。结论该方法简单易行,专属性强,准确性好,可用于益气止血颗粒中盐酸小檗碱、盐酸巴马汀和盐酸药根碱的含量测定及质量标准中功劳叶的质量控制。Objective To develop a method for the determination of berberine hydrochloride, palmatine hydrochloride and jatrorrhizine hydrochloride in Yiqi Zhixue Granules. Methods The samples were extracted by ultrasonication with methanol for 30 rain, and an ion pair RP - HPLC method was applied to determine three kinds of alkaloids. The column of C18 with temperature at 30℃ was used to separate the target components, the mobile phase consisted of the mixed solution of 0. 01 mol/L sodium -heptanesulfonate solution and equal volume of 0. 01 mol/L potassium dihydrogen phosphate solution(pH being adjusted at 3.1 with phosphoric acid) combined with acetonitfile (70 : 30), the flow rate was 1.0 mL/min, and the detection wavelength was at 345 nm. Results Three kinds of alkaloids were separated perfectly, the average recoveries( n = 6)were 100.95 % (RSD = 2. 10 % ) for berberine chloride, 102. 14 % (RSD = 2. 29 % ) for pal- matine chloride, and 100. 71% (RSD = 2. 65 % ) for jatrorrhizine chloride. Conclusion The developed method is demonstrated to be simple, specific and accurate, which can be used to determine the contents of berberine chloride, palmatine chloride and jatrorrhizine chloride in Yiqi Zhixue Granula, and to control the quality of Folium Mahoniae in Yiqi Zhixue Granules.
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