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七味清胰颗粒中大黄的定性鉴别及定量测定

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本研究旨在建立吉林大学中日联谊医院院内制剂七味清胰颗粒中大黄的鉴别和大黄总蒽醌的含量测定方法.试验采用TLC对七味清胰颗粒中的大黄进行定性鉴别;采用HPLC分别测定颗粒中大黄素、芦荟大黄素、大黄酸、大黄素甲醚、大黄酚的含量,流动相为甲醇-0.1%磷酸水(78∶22),流速为1.0 mL/min,色谱柱为Shim-packGWS-C18柱(250 mm×4.6 mm,5 μm),柱温为25℃,进样量为10μL.七味清胰颗粒中大黄的薄层色谱鉴别专属性强,斑点清晰,阴性对照无干扰.大黄素的线性关系在0.807~4.794 μg/mL浓度范围内良好(R2=0.999 7);芦荟大黄素的线性关系在7.99~47.94μg/mL浓度范围内良好(R2=0.999 8);大黄酸的线性关系在2.0~12.0μg/mL浓度范围内良好(R2=0.9999);大黄素甲醚的线性关系在2.025~12.150μg/mL浓度范围内良好(R2=0.999 8);大黄酚的线性关系在4.015~24.090 μg/mL浓度范围内良好(R2=0.999 6);在精密度试验中,大黄素、芦荟大黄素、大黄酸、大黄素甲醚、大黄酚峰面积RSD值分别为0.24%、0.50%、0.46%、0.41%、1.27%;稳定性试验显示大黄素、芦荟大黄素、大黄酸、大黄素甲醚、大黄酚峰面积RSD值分别为0.64%、0.93%、1.45%、0.94%、1.56%;重现性试验中大黄素、芦荟大黄素、大黄酸、大黄素甲醚、大黄酚含量的RSD值分别为1.01%、0.78%、0.46%、0.30%、0.61%;加样回收试验显示,大黄素、芦荟大黄素、大黄酸、大黄素甲醚、大黄酚回收率分别为99.35%、99.70%、100.12%、99.73%、100.34%;三批样品中5个总蒽醌类成分含量分别为1.142 2,1.131 4,1.136 4 mg/g.本研究所建立的方法操作简便、结果准确、重复性好、回收率高,可用于七味清胰颗粒中大黄的定性鉴别及大黄总蒽醌类成分的定量测定.
Qualitative Identification and Quantitative Determination of Rhubarb in Qiwei Qingyi Granules
The aim of this study was to establish a method for identification of Rhubarb and determination of total anthraquinone in Qiwei Qingyi Granules,a hospital preparation of Jilin University.Rhubarb in Qiwei Qingyi granules was qualitatively identified by TLC.The con-tents of emodin,aloe emodin,rhein,emodin methyl ether and chrysophanol in the particles were determined by HPLC.The mobile phase was consisted of methanol-0.1%phosphoric acid water(78:22)at the flow rate of 1.0 mL/min.The chromatography was performed on Shim-packGWS-C18 column(250 mm× 4.6 mm,5 μm),the column temperature was 25 ℃,and the sample size was 10 μL.Rhubarb in Qiwei Qingyi granules was identified by TLC with strong specificity,clear spots and no interference in negative control.Emodin had a good linear relationship in the concentration range of 0.807~4.794 μg/mL(R2=0.999 7).Aloe emodin had a good linear relationship in the con-centration range of 7.99~47.94 μg/mL(R2=0.999 8).Rhein had a good linear relationship in the concentration range of 2.0~12.0 μg/mL(R2=0.999 9).Emodin methyl ether had a good linear relationship in the concentration range of2.025~12.150 μg/mL(R2=0.999 8).Chrysophanol had a good linear relationship in the concentration range of 4.015~24.090 μg/mL(R2=0.999 6).The RSD values of emodin,aloe emodin,rhein,emodin methyl ether and chrysophanol in precision test were 0.24%,0.50%,0.46%,0.41%and 1.27%,respectively(RSD%was less than 2%).The RSD values of emodin,aloe emodin,rhein,emodin methyl ester and chrysophanol in stability test were 0.64%,0.93%,1.45%,0.94%and 1.56%,respectively(RSD%were all less than 2%).The RSD values of emodin,aloe emodin,rhein,emodin methyl ether and chrysophanol in reproducibility tests were 1.01%,0.78%,0.46%,0.30%and 0.61%,respectively(RSD%were all less than 2%).The re-coveries of emodin,aloe emodin,rhein,emodin methyl ether and chrysophanol were 99.35%,99.70%,100.12%,99.73%,100.34%,respec-tively.Total content of five total anthraquinone components in three batches of samples were 1.1422 mg/g,1.1314 mg/g and 1.1364 mg/g,respectively.The method established in this study is simple and accurate,with good repeatability and high recovery rate,and can be used for qualitative identification of Rhubarb and quantitative determination of total anthraquinones in Rhubarb in Qiwei Qingyi Granules.

Qiwei Qingyi Granulethin layer chromatographyhigh performance liquid chromatographyrhubarbcontent determination

蒋倩、高舒琦、高洋、于倩

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吉林大学药学院,吉林 长春 130021

吉林大学中日联谊医院,吉林 长春 130033

七味清胰颗粒 薄层色谱法 高效液相色谱法 大黄 含量测定

吉林省卫生科研人才专项项目

2022SCZ15

2024

特产研究
中国农业科学院特产研究所,中国农学会特产学会

特产研究

CSTPCD
影响因子:0.331
ISSN:1001-4721
年,卷(期):2024.46(5)
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