祛寒逐风颗粒中挥发油提取工艺和包合工艺优化

Optimization of Extraction Technology of Volatile Oil and Inclusion Technology in Quhan Zhufeng Granules

目的:建立祛寒逐风颗粒中藁本内酯的含量测定方法,并优化其中挥发油提取工艺及包合工艺。方法:采用高效液相色谱法测定藁本内酯的含量,色谱柱为Waters C_(18),流动相为甲醇-水(70∶30,V/V),流速为1 mL/min,检测波长为327 nm,柱温为30℃,进样量为10μL;以挥发油得率、藁本内酯含量为考察指标,以浸泡时间、加水量、提取时间为考察因素,采用正交试验设计优化挥发油提取工艺;以包合率、包合物收得率、包合物得油率为考察指标,以挥发油与β-环糊精比例、包合温度、包合时间为考察因素,采用正交试验设计优化挥发油包合工艺。结果:藁本内酯进样量线性范围为0.4～4μg(r=0.999 9);精密度、稳定性、重复性试验的RSD均小于2%(n=6);加样回收率为96.75%～102.03%(RSD=2.06%,n=6)。最优挥发油提取工艺为加入10倍量水(mL/g)、浸泡15 min、提取8 h,所得平均挥发油得率为0.310 7%,平均藁本内酯含量为0.418 0 mg/g;最优挥发油包合工艺为挥发油与β-环糊精比例1∶8(mL/g)、包合温度50℃、包合时间3 h,所得平均包合率为69.43%,平均包合物收得率为58.89%,平均包合物得油率为14.15%。结论:所建含量测定方法操作简便、准确,稳定性较好;优化所得挥发油提取工艺及包合工艺稳定、可行。

OBJECTIVE:To establish the method for content determination of ligustilide and to optimize the extraction technology of volatile oil and inclusion technology in Quhan zhufeng granules.METHODS:HPLC method was adopted.The determination was performed on Waters C18 column with mobile phase consisted of methanol-water(70∶30,V/V)at the flow rate of 1 mL/min.The detection wavelength was set at 327 nm,and the column temperature was 30℃.The sample size was 10μL.Using yield of volatile oil and the content of ligustilide as index,with soaking time,the amount of adding water and extraction time as factors,the extraction technology was optimized by orthogonal test.Using inclusion rate,the yield of inclusion compound and yield of volatile oil as index,with ratio of volatile oil toβ-cyclodextrin,inclusion temperature and inclusion time as factors,the inclusion technology of volatile oil was optimized by orthogonal test.RESULTS:The linear range of ligustilide was 0.4-4μg(r=0.999 9);RSDs of precision,stability and reproducibility tests were all lower than 2%(n=6).The recoveries were 96.75%-102.03%(RSD=2.06%,n=6).The optimal extraction technology of volatile oil included 10-fold water(mL/g),soaking for 15 min,extracting for 8 h.Average yield of volatile oil was 0.310 7%,and average content of ligustilide was 0.418 0 mg/g.The optimal inclusion technology of volatile oil included ratio ofβ-cyclodextrin and volatile oil was 1∶8(mL/g);inclusion temperature was 50℃;inclusion time was 3 h.Average inclusion rate was 69.43%,and the yield of inclusion compound was 58.89%;the yield of volatile oil was 14.15%.CONCLUSIONS:Established determination method is simple,accurate and stable.The optimal extraction technology of volatile oil and inclusion technology are stable and feasible.