成分分析

UPLC-MS/MS法同时测定经典名方实脾散中20个化学成分的含量*

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  • 1.河北中医学院,河北省中药配方颗粒技术创新中心,中药材品质评价与标准化河北省工程研究中心,石家庄 050091;
    2.贵州中医药大学,贵阳 550025
第一作者 Tel:(0311)89926890;E-mail:wsmjm_113@163.com
**Tel:(0311)89926548;E-mail:niuliyingyy@163.com

修回日期: 2022-11-07

  网络出版日期: 2024-06-24

基金资助

*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)

Simultaneous determination of twenty chemical components in Shipi powder by UPLC-MS/MS*

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  • 1. Hebei University of Traditional Chinese Medicine, Hebei Traditional Chinese Medicine Formula Granule Engineering & Technology Innovate Center, Quality Evaluation & Standardization Hebei Province Engineering Research Center of Traditional Chinese Medicine, Shijiazhuang 050091, China;
    2. Guizhou University of Traditional Chinese Medicine, Guiyang 550025, China

Revised date: 2022-11-07

  Online published: 2024-06-24

摘要

目的: 建立UPLC-MS/MS法同时测定实脾散中20个化学成分(槟榔碱、环磷酸腺苷、新绿原酸、绿原酸、隐绿原酸、咖啡酸、甘草苷、苯甲酰新乌头原碱、苯甲酰乌头原碱、异甘草苷、苯甲酰次乌头原碱、甘草素、异甘草素、甘草酸、6-姜辣素、和厚朴酚、木香烃内酯、去氢木香内酯、厚朴酚、白桦脂酸)的含量。方法: 采用岛津Shim-pack GIST C18色谱柱(100 mm×2.1 mm,2 μm),流动相为0.1%甲酸水(A)-乙腈(B),梯度洗脱(0~12 min,2%B→14%B;12~24 min,14%B→51%B;24~26 min,51%B→70%B;26~36 min,70%B;36~37 min,70%B→2%B;37~40 min,2%B),柱温为35 ℃,流速为0.3 mL·min-1,进样量为1 μL;采用电喷雾电离源(ESI源),多重反应监测(MRM)模式正负离子检测。结果: 20个化学成分在测定浓度范围内线性关系良好,相关系数均>0.997 6;精密度、重复性和稳定性良好;平均加样回收率为93.4%~108.7%,RSD≤5.0%。15批样品中槟榔碱、环磷酸腺苷、新绿原酸、绿原酸、隐绿原酸、咖啡酸、甘草苷、苯甲酰新乌头原碱、苯甲酰乌头原碱、异甘草苷、苯甲酰次乌头原碱、甘草素、异甘草素、甘草酸、6-姜辣素、和厚朴酚、木香烃内酯、去氢木香内酯、厚朴酚、白桦脂酸测定结果分别为7 190.26~13 726.74、90.11~301.93、9.65~71.13、102.88~710.98、40.51~179.73、10.90~71.22、3 424.43~27 337.63、508.34~1 276.14、108.27~192.65、95.74~378.92、565.19~1 018.53、106.23~623.42、3.53~16.47、6 104.50~15 933.93、1 047.58~1 750.15、537.91~2 582.74、332.83~581.28、348.22~760.81、350.65~2 189.73、2.06~39.22 μg·g-1结论: 本方法准确灵敏,稳定性和重复性好,可用于实脾散的质量控制。

本文引用格式

麻景梅, 姜晓娅, 麻朝朝, 李琛, 范帅帅, 王鑫国, 牛丽颖 . UPLC-MS/MS法同时测定经典名方实脾散中20个化学成分的含量*[J]. 药物分析杂志, 2023 , 43(3) : 429 -439 . DOI: 10.16155/j.0254-1793.2023.03.09

Abstract

Objective: To establish an ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for the simultaneous determination of twenty chemical components(arecoline hydrobromide, adenosine cyclophosphate, neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, caffeic acid, liquiritin, benzoylmesaconine, benzoylaconitine, isoliquiritin, benzoylhypacoitine, liquiritigenin, isoliquiritigenin, glycyrrhizic acid, 6-gingerol, honokiol, costunolide, dehydrocostus lactone, magnolol, betulinic acid)in Shipi powder. Methods: The separation was performed over 40.0 min on a Shim-pack GIST C18 column(100 mm×2.1 mm,2.0 μm) with a mobile phase consisting of 0.1% formic acid in water and acetonitrile with gradient elution (0-12 min, 2%B→14%B;12-24 min,14%B→51%B;24-26 min,51%B→70%B;26-36 min,70%B;36-37 min,70%B→2%B;37-40 min,2%B) at a flow rate of 0.3 mL·min-1. The column temperature was 35 ℃ and the injection volume was 1 μL. The detection was carried out by electrospray ionization(ESI). Positive and negative electrospray ionizations were performed in multiple reaction monitoring(MRM) mode. Results: All of the analytes showed good linearity(r≥0.997 6) in the tested ranges. The precision, repeatability and stability of the method were good for the twenty chemical components. The average recoveries were in the range of 93.4%-108.7% with relative standard deviations RSD≤5.0%. The contents of arecoline, adenosine cyclophosphate, neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, caffeic acid, liquiritin, benzoylmesaconine, benzoylaconitine, isoliquiritin, benzoylhypacoitine, liquiritigenin, isoliquiritigenin, glycyrrhizic acid, 6-gingerol, honokiol, costunolide, dehydrocostus lactone, magnolol, betulinic acid in 15 bantches of in Shipi powder were 7 190.26-13 726.74, 90.11-301.93, 9.65-71.13, 102.88-710.98, 40.51-179.73, 10.90-71.22, 3 424.43-27 337.63, 508.34-1 276.14, 108.27-192.65, 95.74-378.92, 565.19-1 018.53, 106.23-623.42, 3.53-16.47, 6 104.50-15 933.93, 1 047.58-1 750.15, 537.91-2 582.74, 332.83-581.28, 348.22-760.81, 350.65-2 189.73, 2.06-39.22 μg·g-1. Conclusion: The established method is accurate, stable and reproducible,and can provide a research method for the quality control of Shipi powder.

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