首页|基于HPLC-MS/MS和化学模式识别分析的蒙药那如-3味丸质量评价

基于HPLC-MS/MS和化学模式识别分析的蒙药那如-3味丸质量评价

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目的:基于高效液相色谱-三重四极杆质谱(HPLC-MS/MS)建立同时测定那如-3味丸中9个成分的定量分析方法，结合化学模式识别比较不同批次间质量差异。方法:基于HPLC-MS/MS进行定量分析，色谱柱采用Shim-packGIST-HP C18(2。1 mm×100 mm，3 μm)，流动相甲醇(A)-0。1％甲酸水(B)，流速0。25 mL·min-1，柱温35 ℃，进样量3 μL，正、负离子模式下多反应监测(MRM)方式定量分析16批次那如-3味丸中9个成分含量，并利用微生信科研绘图平台及SIMCA 14。1软件对含量数据进行聚类热图分析、主成分分析(principal component analysis，PCA)和正交偏最小二乘判别分析(orthogonal par-tial least squares discriminant analysis，OPLS-DA)，进而筛选那如-3味丸质量差异标志物。结果:没食子酸、柯里拉京、苯甲酰新乌头原碱、苯甲酰乌头原碱、苯甲酰次乌头原碱、新乌头碱、次乌头碱、乌头碱、胡椒碱在线性范围内呈良好的线性关系(r≥0。999 0)，精密度、稳定性、重复性的RSD均小于3。0％，加样回收率范围在95。91％～102。92％。聚类热图和PCA分析将16批样品分为两大类，OPLS-DA法确定了 6个差异标志物，分别为柯里拉京、苯甲酰新乌头原碱、苯甲酰乌头原碱、苯甲酰次乌头原碱、新乌头碱、乌头碱。结论:所建分析方法稳定、可行，HPLC-MS/MS结合化学计量学分析可全面评价不同厂家、不同批次间那如-3味丸差异，并筛选出差异组分，为该制剂工艺优化及质量评价提供参考。
Quality evaluations of Mongolian medicine Naru-3 Pills based upon HPLC-MS/MS and chemical pattern recognition analysis
OBJECTIVE To establish an HPLC MS/MS method for simultaneous determination of 9 chemical components in Naru-3 Pills and compare the quality variations between different batches of samples by chemometric analysis.METHODS Quantitative analysis was performed on Shim-pack GIST-HP C18(2.1 mm× 100 mm,3 μm)by HPLC MS/MS with a mobile phase of methanol(A)-0.1％formic acid aqueous solution(B).Flow rate was 0.25 mL·min-1,column temperature 35 ℃ and volume of sample injection 3 μL.The contents of 9 components in 16 batches of Naru-3 Pills were quantitatively analyzed by multi-reaction monitoring(MRM)under positive and negative ion modes.The contents data were processed by cluster heat map,principal component analysis(PCA)and orthogonal partial least squares discriminant analysis(OPLS-DA)using bioinformatic platform and SIMCA14.1 software for screening the quality markers of Naru-3 Pills.RESULTS Gallic acid,corilagin,benzoyl-neoaconine,benzoylaconine,benzoylhypaconine,mesaconitine,hypaconitine,aconitine and piperine demonstrated excellent lin-ear relationships in a linear range(r≥0.999 0).Relative standard deviations(RSDs)of precision,stability and reproducibility tests were all under 3.0％with a recovery range of 95.91％—102.92％.The 16 batches of samples were divided into two catego-ries by cluster heat map and PCA analysis.Corilagin,benzoylneoaconine,benzoylaconine,benzoylhypaconine,mesaconitine and aconitine were identified as differential markers by OPLS-DA.CONCLUSION The established analytical method is both stable and feasible.Combining HPLC-MS/MS and chemometrics,it may comprehensively evaluate the variations between different batches of Naru-3 Pills from different manufacturers.And key characteristic components are screened out for guiding the optimiza-tion of production processes and quality supervisions.

Naru-3 PillsHPLC-MS/MSquantitative analysischemical pattern recognition analysisquality evaluation

李君、张谦、王跃武、张微、胡玉霞、王芳、张梦迪、周树宏、王晓琴

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内蒙古医科大学药学院,内蒙古呼和浩特 010110

内蒙古自治区新药筛选工程研究中心,内蒙古呼和浩特 010110

内蒙古医科大学基础医学院,内蒙古呼和浩特 010110

那如-3味丸 高效液相色谱串联三重四级杆质谱 定量分析 化学模式识别 质量评价

内蒙古自治区自然科学基金内蒙古自治区自然科学基金内蒙古自治区高等学校科研项目内蒙古医科大学面上项目内蒙古医科大学蒙药学"一流学科"青年教师科研创新能力提升项目

2022LHQN080012023QN08016NJZY22655YKD2022MS038MYX2023-S05

2024

10.13286/j.1001-5213.2024.11.07

中国医院药学杂志
中国药学会

中国医院药学杂志

CSTPCD北大核心
影响因子：1.198
ISSN：1001-5213
年,卷(期)：2024.44(11)
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