首页|HPLC-MS/MS法同时测定胆木不同部位6个成分的含量

HPLC-MS/MS法同时测定胆木不同部位6个成分的含量

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目的:测定胆木茎、枝和叶中异长春花苷内酰胺、喜果苷、乌檀酰胺C、绿原酸、3,4,5-三甲氧基苯基-1-O-β-呋喃芹糖基(1→2)-β-D-吡喃葡萄糖苷、3,4-二甲氧基苯基-1-O-β-呋喃芹糖基(1→2)-β-D-吡喃葡萄糖苷6个成分的含量.方法:采用 HPLC-MS/MS 法,色谱柱为 Phenomenex Kinete EVO C18 100Å(50 mmx2.1 mm,2.6 μm)柱;流动相为0.5‰甲酸溶液-甲醇,梯度洗脱;流速为0.4 mL/min;柱温为40 ℃;进样量为3 μL;电喷雾离子源,多反应监测负离子模式.结果:异长春花苷内酰胺、喜果苷、乌檀酰胺C、绿原酸、3,4,5-三甲氧基苯基-1-O-β-呋喃芹糖基(1→2)-β-D-吡喃葡萄糖苷、3,4-二甲氧基苯基-1-O-β-呋喃芹糖基(1→2)-β-D-吡喃葡萄糖苷的线性范围分别为0.025~2μg/mL、0.0125~2μg/mL、0.05~2 μg/mL、0.025~2 μg/mL、0.0125~2 μg/mL、0.0125~2 μg/mL(r≥0.9991),精密度、稳定性(24 h)、重复性试验RSD<5.00%,平均加样回收率为95.13%~103.02%(RSD<4.00%).含量测定结果显示6个成分在胆木不同部位中的含量存在较大差异.结论:所建立的方法简便、快速、灵敏,适用于胆木药材中6个成分的同时检测.
Simultaneous Determination of Six Components in Different Parts of Nauclea officinalis by HPLC-MS/MS Method
Objective:To determine the contents of isovincristine lactam,vincosamide,unsantam C,chlorogenic acid,3,4,5-trime-thoxyphenyl-1-O-β-furanosyl(1→2)-β-D-glucopyranoside,3,4-dimethoxy-phenyl-1-O-β-furanosyl(1→2)-β-D-glucopyranoside in the stems,branches and leaves of Nauclea officinalis.Methods:The separation was performed on a Phenomenex Kinete EVO C18 100 Å(50 mmx2.1 mm,2.6 μm)column by HPLC-MS/MS.The mobile phase was 0.5‰ formic acid solution and methanol with gradient elu-tion,flow rate was 0.4 mL/min,column temperature was 40 ℃,injection volume was 3 μL,electrospray ion source,multi-reaction moni-toring negative ion mode.Results:The linear ranges of above six components were 0.025 to 2 μg/mL,0.0125 to 2 μg/mL,0.05 to 2μg/mL,0.025 to 2 μg/mL,0.0125 to 2 μg/mL,0.0125 to 2 μg/mL(r≥0.9991).The RSD of precision,stability(24 h)and repeat-ability tests was less than 5.00%,and the average recoveries were 95.13%to 103.02%(RSD<4.00%).The results of content determi-nation showed that the content of six components in different parts of Nauclea officinalis was different.Conclusion:The established meth-od is simple,rapid and sensitive,and is suitable for the simultaneous determination of the six components in Nauclea officinalis.

Nauclea officinalis Pierre.ex PitardChemical constituentsContent determinationHigh performance liquid chroma-tography-tandem mass spectrometry

贾安、黄小强、茹国华、吴毓皇、明古旭、李永辉

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黄河科技学院医学院,河南 郑州 450063

河南大学药学院,河南 开封 475004

海南医学院药学院/海南省热带药用植物研究开发重点实验室,海南 海口 570100

胆木 化学成分 含量测定 高效液相色谱-串联质谱法

国家自然科学基金河南省研究生教育改革与质量提升工程项目

82160826YJS2023JD68

2024

中药材
国家食品药品监督管理局,中药材信息中心站

中药材

CSTPCD北大核心
影响因子:0.913
ISSN:1001-4454
年,卷(期):2024.47(2)