HPLC双波长法同时测定2种枳术丸中8种有效成分的含量  

Simultaneous determination of eight components in two kinds of Zhizhu pills using double-wavelength HPLC

作　　者：宋志前[1] 董运茁 张婷[3] 杜智勇[1,4] 王淳[1] 甘嘉荷 刘振丽[1] SONG Zhi-qian DONG Yun-zhuo ZHANG Ting DU Zhi-yong WANG Chun GAN Jia-he LIU Zhen-li(The Institute of Basic Theory of Chinese Medicine, China Academy of Chinese Medical Sciences, Beijing 100700, China College of Pharmaceutical and Biotechnology, Tianjin University, Tianjian 300072 Guang＇ anmen Hospital, China Academy of Chinese Medical Sciences, Beijing 100053, China Peking University School of Pharmaceutical Sciences, Beijing 100191, China)

机构地区：[1]中国中医科学院中医基础理论研究所,北京100700 [2]天津大学药物科学与技术学院,天津300072 [3]中国中医科学院广安门医院,北京100053 [4]北京大学药学院,北京100191

出　　处：《药物分析杂志》2016年第10期1715-1721,共7页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立HPLC双波长法同时测定酸橙枳术丸和甜橙枳术丸中多成分的含量,为质量评价提供依据。方法:采用Agilent XDB-C(18)(4.6 mm×250 mm,5μm)色谱柱,以0.01%磷酸二氢钠水溶液(A)-乙腈(B)为流动相,梯度洗脱(0~5 min,5%B;5~7 min,5%B→10%B;7~10 min,10%B→16%B;10~25 min,16%B→18%B;25~42 min,18%B→35%B;42~55 min,35%B→58%B;55~65 min,58%B;65~75 min,58%B→100%B;75~85 min,100%B),流速1mL·min^(-1),柱温30℃,检测波长283nm测定芸香柚皮苷、柚皮苷、橙皮苷、新橙皮苷和白术内酯Ⅰ含量,220 nm测定白术内酯Ⅱ、白术内酯Ⅲ和苍术酮含量。结果:苍术酮不稳定,制备的供试品溶液应避光放置,并在制备后6h内完成检测;各成分在一定范围内线性关系良好;平均回收率介于99.14%~102.6%,RSD均小于3%。酸橙枳术丸中检测到8种待测成分,而甜橙枳术丸中没有检测到柚皮苷与新橙皮苷。结论:经方法学验证,本方法可为枳术丸质量控制提供依据。Objective：To establish a double-wavelength HPLC method for simultaneous determination of eight main compounds in Citrus aurantium L- Zhizhu pills and C.sinensis Osbeck- Zhizhu pills.Methods：The separation was performed on an Agilent XDB- C18（4.6 mm×250 mm,5 μm）column.The mobile phase consisted of 0.01%sodium dihydrogen phosphate water solution（A）- acetonitrile（B） with gradient elute（0- 5 min,5%B;5- 7 min,5%B → 10%B;7-10 min,10%B → 16%B;10-25 min,16%B → 18%B;25-42 min,18%B → 35%B;42- 55 min,35%B → 58%B;55- 65 min,58%B;65- 75 min,58%B → 100%B;75- 85 min,100%B）at a flow rate of1 mL · min-1.The column temperature was 30 ℃.The detection wavelength was 283 nm for narirutin,naringin,hesperidin,neohesperidin and atractylendide I,and 220 nm for atractylenolide Ⅱ,atractylendide Ⅲ and atractylon.Results：The determination should be completed within 6 h after the sannple solution was prepared due to the instability of atractylon.All the compounds had good linearity in the defined ranges and the RSDs of recoveries（99.14%-102.6%）of them were below 3%.respectively.All of the eight compounds were determined in Citrus aurantium L- Zhizhu pills,while naringin and hesperidin were not detected in C.sinensis Osbeck- Zhizhu pill.Conclusion：The established method can be applied to quality contrd of Zhizhu pills according to the methoddogy validation.

关 键 词：酸橙枳术丸 甜橙枳术丸 炒枳实 麸炒白术 芸香柚皮苷 柚皮苷 橙皮苷 新橙皮苷 白术内酯 苍术酮 中成药多组分测定 高效液相色谱双波长法 

分 类 号：R917[医药卫生—药物分析学]