药学学报, 2021, 56(10): 2835-2840
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.
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/MS[J]. Acta Pharmaceutica Sinica, 2021, 56(10): 2835-2840.

UPLC-MS/MS法同时测定橘红中7个成分的含量
范帅帅1, 任海波1, 杨梦婷1, 王鑫国1,2,3,4, 牛丽颖1,2,3,4*
1. 河北中医学院, 河北 石家庄 050091;
2. 河北省中药配方颗粒技术创新中心, 河北 石家庄 050091;
3. 河北省中药材品质评价与标准化工程研究中心, 河北 石家庄 050091;
4. 河北省高校中药配方颗粒应用技术研发中心, 河北 石家庄 050091
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。
关键词:    橘红      UPLC-MS/MS      含量测定      质量控制     
Simultaneous determination of seven components in Citri Exocarpium Rubrum by UPLC-MS/MS
FAN Shuai-shuai1, REN Hai-bo1, YANG Meng-ting1, WANG Xin-guo1,2,3,4, NIU Li-ying1,2,3,4*
1. Hebei University of Chinese Medicine, Shijiazhuang 050091, China;
2. Hebei TCM Formula Granule Innovation Center, Shijiazhuang 050091, China;
3. Hebei TCM Quality Evaluation and Standardization Engineering Research Center, Shijiazhuang 050091, China;
4. TCM Formula Granule Research Center of Hebei Province University, Shijiazhuang 050091, China
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.
Key words:    Citri Exocarpium Rubrum    UPLC-MS/MS    content determination    quality control   
收稿日期: 2021-03-30
DOI: 10.16438/j.0513-4870.2021-0460
基金项目: 中央引导地方科技发展资金项目(206Z2501G);河北省重点研发计划项目(20372502D);河北省自然科学基金资助项目(H2019423050).
通讯作者: 牛丽颖,Tel:86-311-89926548,E-mail:niuliyingyy@163.com
Email: niuliyingyy@163.com
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