中国试验方剂学杂志.DOC

RP - HPLC双波长切换法同时测定复方酸枣仁颗粒中芒果苷和斯皮诺素的含量 田笑菲，李清，梁可，刘莉，陈晓辉，毕开顺( (沈阳药科大学 药学院辽宁 沈阳 110016250 mm × 4.6 mm，5 μm· min -1；柱温30 ℃。结果 在上述色谱条件下，测得芒果苷和斯皮诺素分别在4.320 × 10 -3 ~ 5.200 × 10 -2 mg · mL -1 ( r = 0.9994 ) 和5.200 × 10 -3 ~ 1.040 × 10-1 mg · mL-1 ( r = 0.9997 ) 范围内线性关系良好；芒果苷和斯皮诺素的平均回收率 ( n = 9 )分别为94.6%（ RSD = 1.9 %）和95.1%( RSD = 2.3 % ) 。结论 本法操作简便，准确，重现性良好，可用于复方酸枣仁颗粒的质量控制。 关键词：复方酸枣仁颗粒；芒果苷；斯皮诺素 RP - HPLC simultaneous determination of mangiferin and spinosin in Ziziphus Jujuba Mill Granules under double UV wavelengths Tian xiao-fei, Li qing, Chen xiao-hui, Bi kai-shun* Abstract： To develop a RP-HPLC method for determination of mangiferin and spinosin in Ziziphus Jujuba Mill Granules. METHODS Samples were purified by Liquid –Liquid extraction. Hypersil C18 ( 250 mm × 4.6 mm，5μm ) column was used. The mobile hase consisted of acetonitrile and water with 1% glacial acetic acid; the flow rate was 1.0 mL · min -1. Detection wavelengths were set at 258 nm, and switched to 335 nm at 25 min. RESULTS The linear response ranges were 4.320 × 10 -3 ~ 5.200 × 10 2 mg · mL -1 ( r = 0.9994 ) and 5.200 × 10 -3 ~ 1.040 × 10 -1 mg · mL -1 ( r = 0.9997 ) for mangiferin and spinosin respectively. The average recoveries ( n = 9 ) of these compounds were 94.6 % ( RSD = 1.9 % ) and 95.1 % ( RSD = 2.3 %) respectively. CONCLUSION A simple, accurate and reproducible method is provided for simultaneous determination of mangiferin and spinosin in Ziziphus Jujuba Mill Granules by RP - HPLC. KEY - WORDS : Ziziphus Jujuba Mill Granules; Mangiferin; Spinosin 1 前言 复方酸枣仁颗粒是根据古方酸枣仁汤，采用现代科学方法精制而成，由酸枣仁、川芎、知母、茯苓、甘草5味中药组成，具有养血安神，清热除烦的功效。酸枣仁养肝血、安心神为君药；知母滋阴降火、清热除烦，茯苓宁心安神，共为臣药；川芎调血养肝，为佐药；甘草和中缓肝，为使药。现代药理研究表明，酸枣仁汤中黄酮类成分和多糖类成分在抗焦虑方面有一定的协同作用，其与抗焦虑作用关系最为密切[1]；君药酸枣仁中黄酮类成分斯皮诺素具有重要的镇静、催眠作用[2]；臣药知母中黄酮成分芒果苷具有明显的镇静利胆作用[3]，斯皮诺素、芒果苷均为复方中重要的药效成分，并在复方制剂中含量较大。目前，对于酸枣仁汤及相关制剂有效成分测定多集中于酸枣仁中的酸枣仁皂苷A或B[4,5]， 也有对于酸枣仁中的黄酮类成分和皂苷类成分的同时含量测定[6], 还有采用GC-MC对酸枣仁汤及主要单味成分的超临界流体萃取物的成分进行分析，并对酸枣仁炒前炒后的脂肪油成分进行了比较[7]，发现炒后酸枣仁损失了部分脂肪油类成分；另有文献报道测定酸枣仁浓