高等学校化学学报 ›› 2011, Vol. 32 ›› Issue (12): 2752.

• 研究论文 • 上一篇    下一篇

离子液体均匀提取-高效液相色谱法测定参附注射液中4种单酯型乌头碱的含量

杨瑞杰1,李绪文2,张培旭1,姚华1,睢大筼3,金永日1   

  1. 1. 吉林大学化学学院
    2. 吉林大学化学学院分析化学系
    3. 吉林大学药学院
  • 收稿日期:2011-05-20 修回日期:2011-07-26 出版日期:2011-12-10 发布日期:2011-11-25
  • 通讯作者: 金永日 E-mail:jinyr@jlu.edu.cn

Determination of four kinds of Monoester-diterpenoid aconines in SHEN-FU injection by homogeneous lonic liquid microextraction high-performance liquid chromatography

  • Received:2011-05-20 Revised:2011-07-26 Online:2011-12-10 Published:2011-11-25

摘要:

摘要 采用离子液体均匀提取-高效液相色谱法测定了参附注射液中苯甲酰乌头碱(BA)、苯甲酰新乌头碱(BM)、苯甲酰次乌头碱(BH)和苯甲酰脱氧乌头碱(BD)的含量,通过优化离子液体的用量,样品溶液的pH值,提取时间和盐浓度等参数,确定最佳提取条件为:pH为中性,盐浓度为5%,采用0.058g的[C6Mim][ BF4]和0.26g的 NH4PF6作为提取剂,提取1min,可有效地将目标物从5mL注射液中提取出来。在此实验条件下测得四种单酯型乌头碱的检测限分别为45.5(BM),19.8(BA),26.3(BH)和12.2(BD)μg L-1,对参附注射液样品进行分析,加样回收率范围在93.74-107.91%,RSD值均小于4.34%。

关键词: 单酯型乌头碱, 参附注射液, 离子液体, 高效液相色谱

Abstract:

Abstract The determination of benzoylaconine(BA), benzoylmesaconine(BM), benzoylhypaconine(BH) and benzoyldeoxyaconine(BD) in SHEN-FU injection baced on homogeneous lonic liquid microextraction coupled with high-performance liquid chromatographic separation was described. The experimental parameters including volume of ionic liquid, pH, extraction time and salt concentration were optimizated, when 0.058g [C6Mim][ BF4] and 0.26g NH4PF6 were used as extraction solvent, the target compounds can be extracted from 5mL of injection, the extraction time is 1 min,neutral and the concentration of NaCl is 5%.The detection limits for BA,BM,BH and BD were 45.5,19.8,26.3 and 12.2,respectively. The recoveries of the analytes ranged from 93.74 to 107.91% and relative standard deviations were lower than 4.34%.

Key words: Monoester-diterpenoid aconines, SHEN-FU injection, Lonic liquid, High-performance liquid chromatography

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