中药参姜止痢合剂主要成分含量检测标准研究

doi:10.16431/j.cnki.1671-7236.2023.08.040

摘要/Abstract

摘要： 【目的】建立中药复方参姜止痢合剂的鉴别和含量测定分析方法,为制剂的质量标准提供依据。【方法】采用薄层色谱法(TLC)对参姜止痢合剂中的苦参、干姜做定性鉴别研究;使用高效液相色谱法(HPLC)对参姜止痢合剂中苦参碱、氧化苦参碱进行定量研究。【结果】TLC结果显示,参姜止痢合剂中的苦参、干姜薄层色谱图中供试样品的斑点清晰,与其对应的对照品或对照药材在薄层板相同位置显示一致斑点,阴性对照样品不显示特征斑点。HPLC结果显示,液相色谱图中苦参碱和氧化苦参碱峰型良好,苦参碱在5~100 μg/mL(R²=0.9999)、氧化苦参碱在5~100 μg/mL (R²=0.9999)范围内线性关系良好;仪器精密度测试中相对标准偏差(RSD)值(n=6)为1.56%,说明该套仪器精密度良好,可满足后续含量测定的要求;在样品溶液制备好后0、6、12、24、36、48 h各进样一针,计算RSD(n=6)为2.25%,表明供试品溶液中苦参碱和氧化苦参碱总含量在室温下于48 h内保持稳定;重复性试验结果RSD(n=6)为2.47%,表明样品制备方法重复性良好;苦参碱和氧化苦参碱总含量平均加样回收率为99.17%,RSD(n=6)为2.84%。【结论】本试验建立的参姜止痢合剂的定性及定量分析方法重现性好,结果准确可靠,可对参姜止痢合剂中苦参和干姜进行鉴别,对苦参碱和氧化苦参碱含量进行测定,有效控制其质量。

关键词: 参姜止痢合剂; 质量标准; 薄层色谱; 高效液相色谱

Abstract: 【Objective】 This study was aimed to establish a method for the identification and content determination of Shenjiang Zhili mixture,and to provide a basis for the quality standard of the preparation.【Method】 Thin-layer chromatography (TLC) was used to analyze the Sophora flavescens and Zingiberis Rhizoma for qualitative identification research,and high performance liquid chromatography (HPLC) method was utilized to determine the content of matrine and oxymatrine. 【Result】 TLC results showed that the spots of the test samples in the TLC of Sophora flavescens and Zingiberis Rhizoma were clear,and the corresponding reference substances showed consistent spots in the same position on the TLC plate,while the negative control samples did not show characteristic spots. HPLC results showed that matrine and oxymatrine had good chromatogram peaks. The linear range of matrine from 5 to 100 μg/mL (R²=0.9999) and oxymatrine from 5 to 100 μg/mL (R²=0.9999) were good. The relative standard deviation (RSD) value (n=6) of the instrument precision test was 1.56%,indicating that the precision of the instrument was good and could meet the requirements of the subsequent content determination.At 0,6,12,24,36 and 48 h after the preparation of the sample solution,the calculated RSD (n=6) was 2.25%,indicating that the total content of matrine and oxymatrine in the sample solution remained stable at room temperature for 48 h. Reproducibility test results RSD (n=6) was 2.47%,indicating good reproducibility of the sample preparation method. The average recovery of total matrine and oxymatrine was 99.17%,RSD (n=6) was 2.84%. 【Conclusion】 The results showed that the reproducibility of qualitative and quantitative analysis methods of Shenjiang Zhili mixture was good,the results were accurate and reliable,and it could be used to identify Sophora flavescens and Zingiberis Rhizoma in Shenjiang Zhili mixture and to determine matrine and oxymatrine content,so as to effectively control the quality of matrine.

Key words: Shenjiang Zhili mixture; quality standard; thin layer chromatography; high performance liquid chromatography

中图分类号:

S853.74

刘莲, 郭志廷, 张康, 张凯, 张景艳, 王磊, 李建喜. 中药参姜止痢合剂主要成分含量检测标准研究[J]. 中国畜牧兽医, 2023, 50(8): 3421-3429.

LIU Lian, GUO Zhiting, ZHANG Kang, ZHANG Kai, ZHANG Jingyan, WANG Lei, LI Jianxi. Study on Quality Standard for the Main Components of Traditional Chinese Medicine of Shenjiang Zhili Mixture[J]. China Animal Husbandry and Veterinary Medicine, 2023, 50(8): 3421-3429.

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