中国试验方剂学杂志.docVIP

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，毕开顺基金项目： 基金项目：国家重大新药创制科技重大专项（2009ZX09301-012） 作者：田笑菲，在读硕士研究生，从事中药复方制剂质量标准研究，Tel: 024E-mail: sophietian0512@ 通讯作者：*毕开顺，教授，博士生导师，从事中药化学模式识别、指纹图谱、中药药效物质基础和质量标准研究等。Tel: 024Email: bikaishun@ (沈阳药科大学 药学院，辽宁 沈阳 110016) 摘要：目的 建立复方酸枣仁颗粒中芒果苷和斯皮诺素含量测定的反相高效液相色谱方法。方法 采用液-液萃取法纯化样品。 采用Hypersil C18色谱柱 ( 250 mm × 4.6 mm，5 μm )，以乙腈-1%冰醋酸水系统作为流动相，梯度洗脱；波长检测程序：0 - 25 min，258 nm，25 - 35 min，335 nm；流速1.0 mL · 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 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： OBJECTIVE 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 phase 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