醋五味子配方颗粒及其原料药材饮片中3个木脂素成分的含量测定

Content Determination of Three Lignans in Cuwuweizi(Schisandrae Chinensis Fructus Processed with Vinegar)Granules,Its Raw Material,and Prepared Pieces for Decoction

目的:建立醋五味子配方颗粒及其原料药材、饮片中五味子醇甲、五味子醇乙、当归酰基戈米辛H的含量测定方法,并分析各成分从药材、饮片至配方颗粒的变化。方法:采用高效液相色谱法(HPLC)进行含量测定。色谱柱为Agilent ZORBAX SB-C_(18),流动相为乙腈-水梯度洗脱,柱温为30℃,流速为1.0 mL·min^(-1),检测波长为220 nm,进样量为10μL。结果:五味子醇甲、五味子醇乙、当归酰基戈米辛H检测的线性范围(按进样质量计)分别为0.030~0.380、0.016~0.195、0.009~0.115μg(r>0.999);精密度、稳定性(24 h)、重复性试验的RSD均小于2%;药材、饮片及配方颗粒中,各成分的加样回收率均为98%~102%且RSD均小于2%;五味子中3个成分的质量分数分别为0.44%~0.88%、0.11%~0.44%、0.07%~0.14%,醋五味子中3个成分的质量分数分别为0.48%~0.91%、0.13%~0.47%、0.09%~0.15%,醋五味子配方颗粒中3个成分的质量分数分别为0.15%~0.36%、0.02%~0.16%、0.02%~0.06%。结论:建立了同时测定醋五味子配方颗粒及原料药材、饮片中五味子醇甲、五味子醇乙、当归酰基戈米辛H含量测定方法,该方法分析时间短、专属性强、准确度高,可用于醋五味子配方颗粒从原料到成品的质量评价。

Objective:To establish a high-performance liquid chromatography(HPLC)method for the determination of schisandrin,schisandrol B,angeloylgomisin H in Cuwuweizi Granules(CG),its raw material(RM),and prepared pieces for decoction(PP)and analyze the content changes of the three lignans from RM to PP and CG.Methods:HPLC conditions are as follows:Agilent ZORBAX SB-C_(18)column,gradient elution with acetonitrile-water for gradient elution,flow rate of 1.0 mL·min^(-1),column temperature of 30℃,injection volume of 10μL,and detection wavelength of 220 nm.Results:The linear ranges of the three lignans were 0.030-0.380,0.016-0.195,and 0.009-0.115μg(r>0.999),respectively.The RSDs of precision,stability(24 h),and reproducibility tests were all lower than 2%.The recoveries of the three lignans were 98%-102%with RSDs<2%.The content of the three lignans was 0.44%-0.88%,0.11%-0.44%,and 0.07%-0.14%in RM,0.48%-0.91%,0.13%-0.47%,and 0.09%-0.15%in PP,and 0.15%-0.36%,0.02%-0.16%,and 0.02%-0.06%in CG,respectively.Conclusion:A method was established for the simultaneous determination of schisandrin,schisandrol B,and angeloylgomisin H in CG,RM,and PP.With high specificity,reproducibility,stability,and short time,it can provide a methodological reference for the quality evaluation of CG(from raw materials to finished products).