丁香配方颗粒中挥发油的测定及其质量控制
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摘要
目的:测定丁香配方颗粒中挥发油的含量并尝试建立其质量控制的方法。方法:采用挥发油测定器对丁香总挥发油含量进行测定,以TLC法对其中的挥发性成分进行薄层鉴别,并通过HPLC测定丁香配方颗粒中丁香酚的含量。结果:总挥发油提取过程中二甲苯加入量为1. 5 ml,提取时间为4 h时,其提取率最高,批间平均提取率为12. 24 ml·g~(-1),薄层色谱斑点清晰,分离度好,可较好检出挥发性成分丁香酚;建立的HPLC法表明丁香酚在1. 01～303. 89μg·ml~(-1)范围内呈良好的线性关系(r=1. 000 0),平均加样回收率为100. 65%,RSD为2. 15%(n=9)。结论:所建立的定性、定量方法操作简单、结果准确可靠且重现性好,可有效用于丁香配方颗粒中挥发性成分的质量控制。
Objective: To determine the volatile oil content and establish a quality control method for the volatile components in Caryophylli Flos formula granule. Methods: The total volatile oil content was determined with a volatile oil analyzer. A TLC method was used to identify the volatile components and the others,and the content of eugenol was determined by HPLC. Results: The extraction rate was the highest when the amount of xylene was 1. 5 ml and the extraction time was 4 h,the average extraction rate of interbatch was 12. 24 ml·g~(-1). The TLC spots of components were clear and well-separated,and eugenol was detected out successfully.The HPLC experiment results showed good linearity within the range of 1. 01-303. 89 μg·ml~(-1) (r = 1. 000 0) for eugenol,the average recovery was 100. 65%,and the RSD was 2. 15% (n = 9). Conclusion: The established methods are simple,accurate,reliable and reproducible,and can be effectively used to control the quality of the volatile components in Caryophylli Flos formula granule.
Objective: To determine the volatile oil content and establish a quality control method for the volatile components in Caryophylli Flos formula granule. Methods: The total volatile oil content was determined with a volatile oil analyzer. A TLC method was used to identify the volatile components and the others,and the content of eugenol was determined by HPLC. Results: The extraction rate was the highest when the amount of xylene was 1. 5 ml and the extraction time was 4 h,the average extraction rate of interbatch was 12. 24 ml·g~(-1). The TLC spots of components were clear and well-separated,and eugenol was detected out successfully.The HPLC experiment results showed good linearity within the range of 1. 01-303. 89 μg·ml~(-1) (r = 1. 000 0) for eugenol,the average recovery was 100. 65%,and the RSD was 2. 15% (n = 9). Conclusion: The established methods are simple,accurate,reliable and reproducible,and can be effectively used to control the quality of the volatile components in Caryophylli Flos formula granule.
引文
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2黄妍,姚建标,赖云枫,等.麸炒白术配方颗粒特征图谱及白术内酯Ⅲ含量测定研究[J].中国现代应用药学,2017,34(9):1243-1247
3中国药典[S].2015年版.一部.4,203-204
4杨森.三种丁香花精油的提取、成分分析及抑菌效果检测[D].内蒙古:内蒙古农业大学硕士学位论文,2016
5屠寒.丁香抗氧化活性及质量评价研究[D].武汉:湖北中医药大学硕士学位论文,2017
6杨冰,李婷婷,杨伊涵,等.丁香油抗炎镇痛效果的研究[J].绿色科技,2017,(20):182-185
7桑婷婷.丁香酚通过嗅觉通路对自闭症鼠学习记忆及海马区5-羟色胺表达的影响[D].合肥:安徽医科大学硕士学位论文,2015
8 Ribeiro PA,Miranda-Filho KC,Melo DC,et al.Efficiency of eugenol as anesthetic for the early life stages of Nile tilapia(Oreochromis niloticus)[J].An Acad Bras Cienc,2015,87(1):529-535
9赵婷婷,张彤,项乐源,等.当归、丁香挥发油的促透皮吸收作用[J].中成药,2016,38(9):49-55
10王艳宏,刘书博,王锐,等.中药挥发油促透皮吸收及透皮吸收作用的研究进展[J].中国实验方剂学杂志,2017,23(3):192-199