温阳生肌凝胶中挥发油提取与包合工艺研究

Research on extraction and inclusion technology of volatile oil from Wenyang Shengji gel

目的 以温阳生肌凝胶中君药肉桂挥发油成分桂皮醛为指标成分,建立桂皮醛含量测定方法,优选挥发油提取与包合工艺。方法 2021年3—6月,采用高效液相色谱法测定桂皮醛含量;采用正交试验对挥发油的提取与包合工艺进行优化;采用薄层色谱法与显微鉴别法对包合物进行鉴别。结果 在色谱柱为Agilent C_(18)、流动相为乙腈-水(40∶60)、流速1 mL/min、检测波长290 nm、柱温30℃、进样量10μL的色谱条件下,桂皮醛进样量线性范围为1.136~11.36μg,系统适用性试验良好,精密度、重复性、稳定性及加样回收率试验RSD均<0.2%;最优提取工艺为加8倍量水,浸泡30 min,提取8 h;最优包合工艺为挥发油与β-环糊精比例为1∶10(mL∶g),加水量为5倍,研磨3 h;薄层色谱法提示包合物包合良好。结论 桂皮醛含量测定方法操作简便,优化后的挥发油提取与包合工艺稳定可行,实验结果为温阳生肌凝胶的研究开发提供了技术参数与理论依据。

Objective A method for the determination of cinnamaldehyde was established by using cinnamaldehyde as the index component of volatile oil from Cinnamomum cassia in Wenyang Shengji gel,and optimize the extraction and inclusion process of volatile oil.Methods March to June 2021,high performance liquid chromatography(HPLC) was used to determine the content of cinnamaldehyde.The extraction and inclusion process of volatile oil was optimized by orthogonal design test.The inclusion complexes were identified by thin-layer chromatography(TLC) and microscopic identification method.Results Under chromatographic conditions such as chromatographic column:Agilent C_(18),mobile phase:acetonitrile-water(40:60),flow rate:1 mL/min,detection wavelength:290 nm,column temperature:30℃ and injection volume:10 μL,the linear range of cinnamaldehyde injection volume was 1.136-11.36 μg.The applicability test of the system was good,and the RSD of precision,repeatability,stability and sample recovery test were all <0.2%.The optimum extraction process is as follows:8 fold water,dipping for 0.5 h,extracting for 3 h.The optimum inclusion process is as follows:the ratio of volatile oil to β-cyclodextrin for 1:10(mL:g),5 fold water,and grinding for 3 h.The TLC showed that the inclusion complex was well included.Conclusions The method for determination of cinnamaldehyde is simple,and the optimized extraction and inclusion process of volatile oil is stable and feasible.The experimental results provide technical parameters and theoretical basis for the research and development of Wenyang Shengji gel.