| 摘要: |
| [目的] 建立高效液相串联三重四级杆质谱法(HPLC-MS/MS)测定三叶片中1-脱氧野尻霉素(DNJ)含量的方法。[方法] 采用岛津GL Sciences Inc. NH2色谱柱(150 mm×4.6 mm,5 μm);乙腈(含0.1%甲酸)-0.1%甲酸水(80:20,V:V)为流动相,流速为0.5 mL/min;质谱检测器:采用ESI电离源,离子为164.1/110.2,MRM模式。 [结果] DNJ在61～2 440 μg/L时呈良好的线性关系(r=1.000,n=6),最低检测限为4.26 μg/L,平均加样回收率为105.5%,RSD为7.9%.[结论] 该方法简单、快速、准确,可用于三叶片中DNJ的含量测定。 |
| 关键词: 三叶片 1-脱氧野尻霉素 HPLC-MS/MS 含量测定 |
| DOI：10.11656/j.issn.1673-9043.2013.03.11 |
| 分类号: |
| 基金项目:“重大新药创制”科技重大专项基金项目(2012ZX09 101212). |
|
| Quantitative determination of 1-Deoxynojirimycin in San-Ye tablets by HPLC-MS/MS |
|
JIANG Jia, LIU Hong, LI Xue-ru, HAO Yu, ZHANG De-qin
|
|
Key Laboratory of Pharmacology of Traditional Chinese Medical Formulae (Tianjin University of Traditional Chinese Medicine) Ministry of Education, Tianjin 300193, China
|
| Abstract: |
| [Objective] To develop a HPLC-MS/MS method for determination of 1-Deoxynojirimycin (DNJ) in San-Ye tablets. [Methods] The column was GL Sciences Inc. NH2 (150 mm×4.6 mm, 5 μm), the mobile phase was acetonitrile (cantain 0.1% formic acid)-0.1% formic acid (80:20,V:V), the flow rate was 0.5 mL/min; MS detector: Electrospray ionization (ESI) sources was applied and operated in the position ion mode. Multiple reaction monitoring (MRM) modes with the transition of 164.1/110.2 was used to quantify DNJ. [Results] The linear range of DNJ was 61～2 440 ng/mL (r=1.000, n=6). The lowest limit of detection was 4.26 ng/mL. The average recovery rate was 105.5%, RSD was 7.9%. [Conclusion] The method is simple, rapid, accurate, and can be applied to the determination of DNJ in San-Ye tablets. |
| Key words: San-Ye tablets 1-Deoxynojirimycin HPLC-MS/MS quantitative determination |
