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中国药物评价 ›› 2024, Vol. 41 ›› Issue (4): 289-295.

• 评价技术与方法 • 上一篇    下一篇

大黄通便片中非法成分土大黄苷的定性筛查和定量测定研究

肖小武, 周志强, 洪挺, 杨毅生*, 万林春*   

  1. 江西省药品检验检测研究院,国家药品监督管理局中成药质量评价重点实验室,
         江西省药品与医疗器械质量工程技术研究中心, 江西 南昌 330029
  • 收稿日期:2024-03-07 修回日期:2024-07-16 出版日期:2024-08-28 发布日期:2024-08-28
  • 基金资助:
    江西省重大研发项目“江西省中药饮片炮制规范及我省道地药材品质提升研究(2023BBG7001)”

Study on Qualitative Screening and Quantitative Determination of Rhaponticin in Dahuang Tongbian Tablets

  1. Jiangxi (Provincial Engineering Research Center for Drug and Medical Device Quality,
         NMPA Key Laboratory for Quality Evaluation of Traditional Chinese Medicine,
         Jiangxi Institute For Drug Control, Jiangxi Nanchang 330029,China
  • Received:2024-03-07 Revised:2024-07-16 Online:2024-08-28 Published:2024-08-28

摘要: 目的:建立大黄通便片中土大黄苷的定性筛查和定量测定方法。方法:采用薄层色谱(TLC)法初筛,高效液相色谱(HPLC)法定量测定及超高效液相色谱-质谱联用(UHPLC-MS)法定性确证。结果:TLC法检测结果显示专属性强,耐用性好。HPLC法方法学考察结果显示:土大黄苷质量浓度在2.59~259.6 μg·mL-1范围内呈良好的线性关系(R2=0.999 9);精密度、重复性、稳定性试验RSD均小于2.0%;平均加样回收率为97.89%(RSD=0.61%)。UHPLC-MS/MS法确证结果与TLC、HPLC法结果一致,阳性检出样品与土大黄苷对照品呈现同一保留时间的提取离子对(421.1→258.9,421.1→199.0)。结论:该方法灵敏、准确,可作为大黄通便片中非法成分土大黄苷的检查方法。
     [关键词] 

关键词: font-size:medium, ">大黄通便片;土大黄苷;薄层色谱(TLC);高效液相色谱(HPLC);超高效液相色谱-质谱联用(UHPLC-MS/MS)

Abstract: Objective: To establish a method for the qualitative screening and quantitative determination of rhein in Dahuang Tongbian tablets. Methods: TLC was used for preliminary screening, HPLC was used for quantitative determination, and UHPLC-MS was used for qualitative confirmation. Results: TLC test results showed strong specificity and good durability. HPLC results showed that the mass concentration of rhein showed a good linear relationship in the range of 2.59~259.6 μg·mL-1 (R2=0.999 9). RSDS of precision, repeatability and stability tests were all less than 2.0%. The average recovery was 97.89% (RSD=0.61%). The confirmed results of UHPLC-MS/MS were consistent with TLC and HPLC, and the extracted ion pairs with the same retention time of the positive samples and the control products of rhein (421.1→258.9, 421.1→199.0). Conclusion: The method is sensitive and accurate, and can be used as a method for the detection of illegal components of rhein in Dahuang Tongbian tablets.

Key words: font-size:medium, ">Dahuang Tongbian Tablets;Rhaponticin; Thin Layer Chromatography(TLC); High Performance Liquid Chromatography(HPLC); Ultra-High-Performance Liquid Chromatography Mass Spectrometer(UHPLC-MS/MS)

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