醋五味子配方颗粒的特征图谱建立及5种成分的含量测定
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篇名: 醋五味子配方颗粒的特征图谱建立及5种成分的含量测定
TITLE: Establishment of Characteristic Pattern of Vinegar-processed Schisandra chinensis Formula Granules and Content Determination of 5 Components
摘要: 目的:建立不同产地五味子制醋五味子配方颗粒的特征图谱,并测定其中5种成分的含量。方法:采用高效液相色谱法(HPLC)。色谱柱为AgilentZORBAXSB-C18,流动相为乙腈-水(梯度洗脱),柱温为30℃,流速为1.0mL/min,检测波长为220nm,进样量为10µL。以五味子醇甲为参照,绘制19批醋五味子配方颗粒的HPLC特征图谱;采用《中药色谱指纹图谱相似度评价系统(2012版)》进行相似度评价并确定共有峰;采用相同方法测定五味子醇甲、五味子醇乙、当归酰基戈米辛H、五味子甲素、五味子乙素的含量。结果:19批醋五味子配方颗粒共有8个共有峰,相似度均在0.996以上;共指认五味子醇甲、为五味子醇乙、当归酰基戈米辛H、五味子甲素、五味子乙素等5个共有峰。五味子醇甲、五味子醇乙、当归酰基戈米辛H、五味子甲素、五味子乙素检测进样量的线性范围分别为0.030~0.380、0.016~0.195、0.009~0.115、0.006~0.078、0.011~0.138μg(r>0.999);精密度、稳定性(24h)、重复性试验的RSD均小于2%;平均加样回收率分别为99.84%、99.54%、99.28%、100.03%、100.27%(RSD小于1.4%,n=9)。19批样品中上述5种成分的平均含量分别为0.15%~0.36%、0.02%~0.16%、0.02%~0.06%、0.02%~0.08%、0.08%~0.17%,其中河北产样品S18、S19中的5种成分总含量较高,S16、S17样品总含量较低,RSD为42%,其余样品(S1~S15)总含量的RSD为12%,低于河北产,以吉林产样品含量较高。结论:所建特征图谱及含量测定方法的专属性强、重复性好,可用于评价醋五味子配方颗粒的质量;辽宁、吉林、黑龙江等3省产五味子制醋五味子配方颗粒的总含量波动较河北省低,以吉林省产质量最佳。
ABSTRACT: OBJECTIVE:To establ ish characteristic pattern of vinegar-processed product of Schisandra chinensis formula granules from different habitats ,and to determine the contents of 5 components. METHODS :HPLC method was adopted. The determination was performed on Agilent ZORBAX SB-C 18 column with mobile phase consisted of acetonitrile-water (gradient elution)at the flow rate of 1.0 mL/min. The column temperature was set at 30 ℃,and detection wavelength was set at 220 nm. The sample size was 10 µL. Using schisandrin as reference ,HPLC characteristic pattern of 19 batches of vinegar-processed S. chinensis formula granules was drawn. The similarity evaluation was performed with Similarity Evaluation System of TCM Chromatographic Fingerprints (2012 edition),and common peaks were confirmed. The contents of schisandrin ,schisandrol, angeloylgomisin H ,schizandrin and deoxyschizandrin were determined by same method. RESULTS :There were 8 common peaks in 19 batches of vinegar-processed S. chinensis formula granules ,and the similarities were all above 0.996;five of them were identified as schisandrin ,schisandrol,angeloylgomisin H ,schizandrin and deoxyschizandrin ,respectively. The linear range of schisandrin,schisandrol,angeloylgomisin H ,schizandrin and deoxyschizandrin were 0.030-0.380,0.016-0.195,0.009-0.115, 0.006-0.078 and 0.011-0.138 μg(r>0.999),respectively. RSDs of precision ,stability(24 h)and reproducibility tests were all lower than 2%. Average recoveries were 99.84%,99.54%,99.28%,100.03%,100.27%(RSD<1.4%,n=9). Average contents of five components in 19 batches of samples were in the range of 0.15%-0.36%,0.02%-0.16%,0.02%-0.06%,0.02%-0.08% and 0.08%-0.17%,respectively;among them ,total contents of five components in sample S 18 and S 19 from Hebei province were relatively high ,while those were relatively low in sample S 16 and S 17(RSD=42%);RSD of total content in other samples (S1-S15)was 12%,and was lower than that of Hebei province ;total content of five components were higher in sample from Jilin province. CONCLUSIONS : Established characteristic pattern and method for the content determination are specific and reproducible,and can be used for the quality evaluation of vinegar-processed S. chinensis formula granules. The total content fluctuation of vinegar-processed product of S. chinensis formula granules from Liaoning ,Jilin and Heilongjiang provinces is lower than that in Hebei province ,and the quality of vinegar-processed Δ 基金项目:国家中药标准化项目(No.ZYB2H-Y-GD-13) *主管中药师 ,硕士 。研究方向 :中药质量标准 。E-mail: S. chinensis formula granules from Jilin province is the best. lzz332@126.com
期刊: 2021年第32卷第12期
作者: 刘子祯,姜蕊,许冬瑾
AUTHORS: LIU Zizhen ,JIANG Rui,XU Dongjin
关键字: 醋五味子;配方颗粒;高效液相色谱法;特征图谱;含量测定
KEYWORDS: Vinegar-processed Schisandra chinensis ;
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