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中国药物评价 ›› 2024, Vol. 41 ›› Issue (3): 204-208.

• 评价技术与方法 • 上一篇    下一篇

液质联用法定性检测熟大黄配方颗粒中的 土大黄苷和番泻苷A

王劲, 曲国晶   

  1. 菏泽市食品药品检验检测研究院, 山东 菏泽 274000
  • 收稿日期:2024-01-08 修回日期:2024-03-04 出版日期:2024-06-28 发布日期:2024-06-28

Identification of Rhaponticin and Sennoside A in Stewed Rhubarb Granule by HPLC-MS/MS

  1. Heze City Institute for Food and Drug Control, Shandong Heze 274000,China
  • Received:2024-01-08 Revised:2024-03-04 Online:2024-06-28 Published:2024-06-28

摘要: 目的:应用液质联用法定性检测熟大黄配方颗粒中土大黄苷和番泻苷A。方法:采用HPLC-MS/MS法同时检测土大黄苷和番泻苷A,使用Welch UHPLC XB-C18色谱柱( 2.1 mm×150 mm,1.8 μm),采用0.1%甲酸水-甲醇梯度洗脱,柱温35 ℃,流速0.3 mL·min-1,采用ESI离子源,多反应模式(MRM)模式。结果:该方法对土大黄苷和番泻苷A的检出浓度分别为:2.0 ng·mL-1、8.0 ng·mL-1,用该方法检测了山东省内市售的8批熟大黄配方颗粒,均未检出土大黄苷和番泻苷A。结论:该方法专属性强,灵敏度好,能快速定性检查熟大黄配方颗粒中是否含有土大黄苷和番泻苷A,可用于熟大黄(药用大黄)配方颗粒的质量控制。

关键词: font-size:medium, ">熟大黄配方颗粒;土大黄苷;番泻苷A

Abstract: Objective: To found a method for the identification of rhaponticin and sennoside A in Stewed Rhubarb Granule by LC-MS.Methods: An HPLC-MS /MS in MRM mode was adopted. Welch UHPLC XB-C18(2.1 mm×150 mm,1.8 μm) column was applied with methanol-0.1% phosphoric acid solution as the mobile phase.The Liquid phase flow velocity was 0.3 mL·min-1,The temperature of colum was 35 ℃. The MS/MS system was operated by using an electrospray ionization probe. Scan mode was in multiple reaction ion monitoring(MRM) mode. Results: Limits of detection were 2.0 ng·mL-1 for Rhaponticin and 8.0 ng·mL-1 for Sennoside A.Rhaponticin and Sennoside A weren′t found in 8 batches of samples. Conclusion: The method is exclusive and could not only identify the true or false Stewed Rhubarb,but also examine the purity. It′s necessary for the quality control of Stewed Rhubarb Granule.

Key words: font-size:medium, ">Stewed Rhubarb Dispensing Granule;Rhaponticin; Sennoside A

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