UPLC-MS/MS同时测定天麻胶囊中23种成分含量

王发英; 毛菊华; 王伟影

doi:10.13748/j.cnki.issn1007-7693.20232234

UPLC-MS/MS同时测定天麻胶囊中23种成分含量

Simultaneous Determination of 23 Components in Tianma Capsules by UPLC-MS/MS

摘要

摘要:
目的建立UPLC-MS/MS同时测定天麻胶囊中梓醇、天麻素、地黄苷D、哈巴苷、巴利森苷E、巴利森苷B、巴利森苷C、阿魏酸、巴利森苷、紫花前胡苷、β-蜕皮甾酮、二氢欧山芹醇、新乌头碱、次乌头碱、乌头碱、哈巴俄苷、二氢欧山芹醇醋酸酯、藁本内酯、蛇床子素、镰叶芹二醇、二氢欧山芹醇当归酸酯、异欧前胡素、羌活醇23种成分含量的分析方法。
方法 UPLC采用色谱柱为 Agilent Poroshell 120 SB-C₁₈ (2.1 mm×100 mm，1.8 μm)，以甲醇-0.1%甲酸水溶液梯度洗脱，流速为0.3 mL·min⁻¹，柱温35 ℃，进样量为1 μL；质谱法采用三重四级杆质谱，电喷雾离子源、正负离子交替扫描模式，通过多重反应监测进行定量分析。
结果 23种成分在一定范围内均呈现良好线性关系(r>0.99)；精密度、重复性和稳定性良好；平均加样回收率在86.7%~107.4%。
结论该方法同时测定了天麻胶囊中23种成分的含量，方法可行，重现性好，可为天麻胶囊的质量控制提供方法参考。

Abstract:
OBJECTIVE To establish an analytical method for simultaneous determination of contents of 23 components in Tianma capsules, including catalpol, gastrodin, rehmannioside D, harpagide, parishin E, parishin B, parishin C, ferulic acid, parishin, nodakenin, β-ecdysterone, columbianetin, mesaconitine, hypaconitine, aconitine, harpagoside, columbianetin acetate, ligustilide, osthole, falcarindiol, columbianadin, isoimperatorin, notopterol by UPLC-MS/MS.
METHODS The UPLC method was performed on Agilent Poroshell 120 SB-C₁₈ (2.1 mm×100 mm, 1.8 μm), with methanol- 0.1% formic acid as the mobile phase for gradient elution. The column temperature was set at 35 ℃ with flow rate of 0.3 mL·min⁻¹, and the injection volume was 1 μL. Mass spectrometry used the triple quadrupole mass spectrometry, electrospray ionization(ESI) source was applied, and operated in alternating positive and negative mode. The multiple reaction monitoring mode was employed for the quantitative analysis.
RESULTS The 23 components showed good linear relationship within their own ranges(r>0.99)．The method had good precision, repeatability, and stability. The average recoveries were between 86.7%–107.4%.
CONCLUSION This method simultaneously determined the content of 23 components in Tianma capsules. The method is feasible and has good reproducibility, which can provide a reference for the quality control of Tianma capsules.

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