王怜星, 娄佳, 孙梦冉, 徐晓艳, 王宇, 王跃飞, 杨文志. 基于串联质谱多重反应监测的进口血竭与国产龙血竭中17种成分的含量测定J. 药学学报, 2025, 60(7): 2316-2323. DOI: 10.16438/j.0513-4870.2025-0188
引用本文: 王怜星, 娄佳, 孙梦冉, 徐晓艳, 王宇, 王跃飞, 杨文志. 基于串联质谱多重反应监测的进口血竭与国产龙血竭中17种成分的含量测定J. 药学学报, 2025, 60(7): 2316-2323. DOI: 10.16438/j.0513-4870.2025-0188
WANG Lian-xing, LOU Jia, SUN Meng-ran, XU Xiao-yan, WANG Yu, WANG Yue-fei, YANG Wen-zhi. Content determination of seventeen components in Dragon's Blood and Chinese Dragon's Blood based on multiple reaction monitoring tandem mass spectrometryJ. Acta Pharmaceutica Sinica, 2025, 60(7): 2316-2323. DOI: 10.16438/j.0513-4870.2025-0188
Citation: WANG Lian-xing, LOU Jia, SUN Meng-ran, XU Xiao-yan, WANG Yu, WANG Yue-fei, YANG Wen-zhi. Content determination of seventeen components in Dragon's Blood and Chinese Dragon's Blood based on multiple reaction monitoring tandem mass spectrometryJ. Acta Pharmaceutica Sinica, 2025, 60(7): 2316-2323. DOI: 10.16438/j.0513-4870.2025-0188

基于串联质谱多重反应监测的进口血竭与国产龙血竭中17种成分的含量测定

Content determination of seventeen components in Dragon's Blood and Chinese Dragon's Blood based on multiple reaction monitoring tandem mass spectrometry

  • 摘要: 为了有效测定进口血竭与国产龙血竭中特征成分的含量, 本研究基于超高效液相色谱-三重四极杆-线性离子阱质谱技术, 构建了多重反应监测方法, 采用ACQUITY UPLC BEH C18色谱柱(2.1 mm × 100 mm, 1.7 μm), 在30 ℃柱温下以0.1%甲酸水-乙腈为流动相、0.3 mL·min-1的流速进行梯度洗脱, 在22 min内同时实现了血竭中6个特征成分与龙血竭中11个特征成分的分离与含量测定。该方法专属性好, 可以快速、高效地测定血竭和龙血竭中共17种特征成分的含量, 各成分均呈现良好的线性关系(R2 > 0.99), 平均加样回收率为93.58%~105.82%。结果表明, 进口血竭中血竭素、(2S)-7-羟基-5-甲氧基黄烷和(2S)-7-羟基-5-甲氧基-6-甲基黄烷等成分含量较高, 国产龙血竭中龙血素B、龙血素D和紫檀芪等成分含量显著, 但不同批次间存在较大差异。这些结果可为血竭和龙血竭药材的质量控制和标准制定提供参考, 同时也可为区分其他相近中药的质量控制研究提供思路。

     

    Abstract: To effectively determine the content of characteristic components in imported Dragon's Blood (DB) and domestic Chinese Dragon's Blood (CDB), this study established a multiple reaction monitoring (MRM) method based on ultra-high performance liquid chromatography-triple quadrupole-linear ion trap mass spectrometry (UHPLC-Q-Trap-MS). Chromatographic separation was achieved using an ACQUITY UPLC BEH C18 column (2.1 mm × 100 mm, 1.7 μm) at 30 ℃ with a mobile phase consisting of 0.1% formic acid aqueous solution and acetonitrile at a flow rate of 0.3 mL·min-1 under gradient elution. The method successfully separated and quantified six characteristic components in DB and eleven in CDB within 22 minutes. The developed approach demonstrated excellent specificity, enabling rapid and efficient determination of 17 components. All analytes exhibited strong linearity (R2 > 0.99), and the average recovery rate was 93.58%-105.82%. Results revealed that imported Dragon's Blood contained higher levels of dracorhodin, (2S)-5-methoxyflavan-7-ol and (2S)-5-methoxy-6-methylflavan-7-ol, while domestic Chinese Dragon's Blood was rich in loureirin B, loureirin D and pterostilbene, albeit with significant variations among different batches. These findings provide critical references for quality control and standardization of DB and CDB, as well as the insights for distinguishing similar traditional Chinese medicines.

     

/

返回文章
返回