正交试验法优选蜜升麻的炮制工艺研究

Study on the Processing Technology of Honey-Fried Shengma(Cimicifugae Rhizoma)by Orthogonal Test

目的:探究蜜升麻的最佳炮制工艺。方法:采用高效液相色谱(HPLC)法测定蜜升麻中的异阿魏酸含量,色谱柱为Syncronis C18(250 mm×4.6 mm,5μm),流动相为甲醇-0.1%磷酸水(75∶25),流速为1.0 mL/min,柱温为30℃,检测波长为321 nm,进样量为10μL;采用正交试验法,以加热温度、加热时间、闷润时间作为考察因素,每一因素设4个水平,以蜜升麻中的异阿魏酸含量、性状外观评分的综合评分为指标进行考察。结果:异阿魏酸的线性范围为0.81~202.40μg/mL(r=0.9998),精密度、稳定性、重复性试验RSD值均小于2%,异阿魏酸的平均加样回收率为101.50%(RSD=1.66%);加热温度对试验结果具有显著影响(P<0.05),加热时间、闷润时间对试验结果影响不显著(P>0.05)。蜜升麻最佳炮制工艺为加热温度100℃、加热时间90 s、闷润时间90 min。结论:该炮制方法操作简便,工艺稳定可靠,可用于蜜升麻的炮制生产。

Objective:To explore the best processing technology of honey-fried Shengma(Cimicifugae Rhizoma).Methods:The content of isoferulic acid in honey-fried Shengma(Cimicifugae Rhizoma)was determined by HPLC.The determination was performed on a Syncronis C18 column(250 mm×4.6 mm,5μm)with mobile phase consisted of methanol-0.1%phosphoric acid water(75∶25)at the flow rate of 1.0 mL/min.The column temperature was 30℃,the detection wavelength was 321 nm and the injection volume was 10μL.The orthogonal test method was used to investigate the heating temperature,heating time and moistening time.Four levels were set for each factor,and the comprehensive score of isoferulic acid content and appearance score of honey-fried Shengma(Cimicifugae Rhizoma)was used as the index.Results:The linear range of isoferulic acid was 0.81-202.40μg/mL(r=0.9998).The RSD values of precision,stability and reproducibility tests were all less than 2%.The average recovery of isoferulic acid was 101.5%(RSD=1.66%).The heating temperature had a significant effect on the test results(P<0.05).The effect of heating time and moistening time had no significant influence on the test results(P>0.05).The optimum processing technology of honey-fried Shengma(Cimicifugae Rhizoma)was heating temperature of 100°C,heating time of 90 s and moistening time of 90 min.Conclusion:The processing method is simple,stable and reliable,and can be used for the processing production of honey-fried Shengma(Cimicifugae Rhizoma).