范帅帅, 任海波, 杨梦婷, 王鑫国, 牛丽颖. UPLC-MS/MS法同时测定橘红中7个成分的含量J. 药学学报, 2021,56(10): 2835-2840. doi: 10.16438/j.0513-4870.2021-0460
引用本文: 范帅帅, 任海波, 杨梦婷, 王鑫国, 牛丽颖. UPLC-MS/MS法同时测定橘红中7个成分的含量J. 药学学报, 2021,56(10): 2835-2840. doi: 10.16438/j.0513-4870.2021-0460
FAN Shuai-shuai, REN Hai-bo, YANG Meng-ting, WANG Xin-guo, NIU Li-ying. Simultaneous determination of seven components in Citri Exocarpium Rubrum by UPLC-MS/MSJ. Acta Pharmaceutica Sinica, 2021,56(10): 2835-2840. doi: 10.16438/j.0513-4870.2021-0460
Citation: FAN Shuai-shuai, REN Hai-bo, YANG Meng-ting, WANG Xin-guo, NIU Li-ying. Simultaneous determination of seven components in Citri Exocarpium Rubrum by UPLC-MS/MSJ. Acta Pharmaceutica Sinica, 2021,56(10): 2835-2840. doi: 10.16438/j.0513-4870.2021-0460

UPLC-MS/MS法同时测定橘红中7个成分的含量

Simultaneous determination of seven components in Citri Exocarpium Rubrum by UPLC-MS/MS

  • 摘要: 建立液质联用(UPLC-MS/MS)方法同时测定橘红中7个成分(绿原酸、芦丁、芸香柚皮苷、橙皮苷、甜橙黄酮、川陈皮素、橘皮素)的含量。采用Shim-pack GIST C18色谱柱(100 mm×2.1 mm,2.0 μm),以乙腈(A)-0.1%甲酸水(B)为流动相,进行梯度洗脱,柱温为30℃,流速为0.4 mL·min-1,进样量为1 μL,分析时间为12 min。采用电喷雾电离源(ESI源),以多重反应监测模式正负离子检测。所测7种化学成分在测定浓度范围内线性关系良好,相关系数均大于0.997 3,精密度、重复性和稳定性良好,平均加样回收率为99.32%~107.75%,RSD ≤ 3.94%。本实验所建立的方法准确灵敏,稳定性和重复性好,可用于橘红药材的质量控制。

     

    Abstract: An ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was established for the simultaneous determination of seven components (chlorogenic acid, rutin, narirutin, hesperidin, sinensetin, nobiletin, tangeretin) in Citri Exocarpium Rubrum. The separation was performed over 12.0 min on a Shim-pack GIST C18 column (100 mm×2.1 mm, 2.0 μm) with a mobile phase consisting of acetonitrile (A) and 0.1% formic acid water solution (B) with gradient elution at a flow rate of 0.4 mL·min-1; the column temperature was 30℃ and the injection volume was 1 μL. Detection was performed on a QTRAP 4500 mass spectrometer equipped with electrospray ionization. Positive and negative electrospray ionization was performed in multiple reaction monitoring mode. All of the analytes showed good linearity (r ≥ 0.997 3) in the tested ranges, with good precision, repeatability and stability for all analytes. The average recoveries were in the range of 99.32%-107.75% with relative standard deviations RSD ≤ 3.94%. The established method is accurate, stable and reproducible, and can provide a research method for the quality control of Citri Exocarpium Rubrum.

     

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