特产研究2024，Vol.46Issue(5)：88-94,7.DOI:10.16720/j.cnki.tcyj.2024.164
七味清胰颗粒中大黄的定性鉴别及定量测定
Qualitative Identification and Quantitative Determination of Rhubarb in Qiwei Qingyi Granules
摘要
Abstract
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.关键词
七味清胰颗粒/薄层色谱法/高效液相色谱法/大黄/含量测定Key words
Qiwei Qingyi Granule/thin layer chromatography/high performance liquid chromatography/rhubarb/content determination分类
医药卫生引用本文复制引用
蒋倩,高舒琦,高洋,于倩..七味清胰颗粒中大黄的定性鉴别及定量测定[J].特产研究,2024,46(5):88-94,7.基金项目
吉林省卫生科研人才专项项目(2022SCZ15) （2022SCZ15）
