| 陈刚,汪生,宫鹏.基于超高效液相色谱 -静电场轨道阱质谱技术的十二味参芍益脑合剂中 12种主要化学成分定量检测研究[J].安徽医药,2023,27(9):1750-1756. |
| 基于超高效液相色谱 -静电场轨道阱质谱技术的十二味参芍益脑合剂中 12种主要化学成分定量检测研究 |
| by ultra-performance liquid chromatography tandem hybrid orbitrap mass spectrometry |
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| DOI：10.3969/j.issn.1009-6469.2023.09.012 |
| 中文关键词: 主成分分析 十二味参芍益脑合剂 超高效液相色谱 -静电场轨道阱质谱 含量测定 平行反应监测 质量控制 |
| 英文关键词: Principal component analysis Shierwei Shenshao Yinao mixture Ultra-performance liquid chromatography tandem hybrid orbitrap mass spectrometry Content determination Parallel reaction monitoring Quality control |
| 基金项目:2021年度安徽省卫生健康委科研重点项目( AHWJ2021a018) |
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| 中文摘要: |
| 目的基于超高效液相色谱 -静电场轨道阱质谱技术，同时测定十二味参芍益脑合剂中 12种主要化学成分(绿原酸、栀子苷、芍药苷、芍药内酯苷、甘草苷、黄芩苷、芹菜素、甘草素、汉黄芩苷、黄芩素、汉黄芩素和千层纸素A)的含量。方法该研究起止时间为 2021年 3月至 2022年 5月。采用 Waters UPLC HSS T3色谱柱( 100 mm × 2.1 mm，1.8 μm)，以乙腈 -0.1%甲酸和 10 mmol/L甲酸铵水溶液为流动相，线性梯度洗脱，流速 0.25 mL/min，柱温 35 ℃，采用电喷雾离子化，平行反应监测离子扫描，以负离子模式检测 16批十二味参芍益脑合剂。结果测定的 12种主要化学成分在检测浓度范围内线性关系良好( r>0.99)，加样回收率范围为 80.58%~112.90%［相对标准差( RSD)<10%］基质效应范围为 76.58%~110.80%(RSD<10%)，进样精密度、重复性、稳定性均符合方法学测定要求。 16批制剂检测结果显示，13批质量相对稳定，其余 3批有一定差异，栀子苷可以作为进一步评价制剂质量的指标。结论该方法专属性强、灵敏度高、重复性好，准确可靠，可用于十二味参芍益脑合剂中 12种主要化学成分的同步含量测定。 |
| 英文摘要: |
| Objective To establish a method for quantification of 12 components (chlorogenic acid, geniposide, paeoniflorin, albiflo-rin, liquiritin, baicalin, apigenin, liquiritigenin, wogonoside, baicalein, wogonin and oroxylin A) in Shierwei Shenshao Yinao mixture by ultra-performance liquid chromatography tandem hybrid orbitrap mass spectrometry (UPLC-Q-Orbitrap-MS) technique.Methods The study started from March 2021 and ended in May 2022. The analysis was performed on a Waters ACQUITY UPLC HSS T3 column (100 mm × 2.1 mm, 1.8 μm) with a mobile phase of acetonitrile-0.1% formic acid and 10 mmol/L ammonium formate aqueous solution forlinearity gradient elution, the flow rate was 0.25 mL/min, and the column temperature was set at 35 ℃. Electrospray ionization sourcewas used for determination in the parallel reaction monitoring mode under anion conditions. Results The 12 targeted compounds showed a satisfying linear relationship within the range of concentration determined (r>0.99), with an average recovery ranged from80.58% to 112.90% (RSD<10%) and the matrix effect ranged from 76.58% to 110.80% (RSD<10%). The precision, repeatability andstability were validated and meet the requirement of quantitation. The content determination of 16 batches of preparation showed thatthe quality of 13 batches was relatively stable, and the other 3 batches were slightly different. Geniposide could be a potential biomark-er in quality evaluation of the preparation.Conclusion This method has high specificity and sensitivity, good repeatability and accura-cy, which could be successfully used for the determination of 12 chemical components in Shierwei Shenshao Yinao mixture. |
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