| 引用本文: |
朱立华,黄生武,沈冰冰,谢谊.UPLC-Q-Exactive-MS/MS测定伤痛宁胶囊中马兜铃酸Ⅰ的含量[J].湖南中医药大学学报,2023,43(8):1415-1420[点击复制] |
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| UPLC-Q-Exactive-MS/MS测定伤痛宁胶囊中马兜铃酸Ⅰ的含量 |
| 朱立华,黄生武,沈冰冰,谢谊 |
| (湖南国华制药有限公司, 湖南 长沙 410013;湖南省中医药研究院, 湖南 长沙 410013) |
| 摘要: |
| 目的 建立UPLC-Q-Exactive-MS/MS测定伤痛宁胶囊中马兜铃酸Ⅰ的含量。方法 采用Hypersil GOLD C18色谱柱（2.1 mm×50 mm，1.9 μm），流动相为乙腈和0.1%甲酸水溶液（含5 mmol/L甲酸铵），梯度洗脱，流速0.5 mL/min，柱温30℃。采用电喷雾离子源正离子模式，进行平行反应监测模式，选择质荷比（m/z）359.0→298.0和359.0→296.0离子对进行监测。结果 马兜铃酸Ⅰ在0.06~0.2 ng范围内线性关系良好（R2=0.999 5），精密度和稳定性的RSD值均小于3%，加样回收率均值为104.1%（RSD=4.29％）。不同批次伤痛宁胶囊样品中马兜铃酸Ⅰ的含量均值为0.000 004 90%，从药材到成品的转移率均值为103.7%，RSD值为19.5%。结论 该方法专属性好，灵敏度高，准确可靠、耐用，可以用于伤痛宁胶囊中马兜铃酸Ⅰ的含量测定。 |
| 关键词: 伤痛宁胶囊 马兜铃酸Ⅰ UPLC Q-Exactive MS/MS 定量分析 |
| DOI：10.3969/j.issn.1674-070X.2023.08.011 |
| 投稿时间：2023-02-04 |
| 基金项目:湖南省科技厅省重点研发计划项目（2016SK2048）。 |
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| Determination of aristolochic acid Ⅰ in Shangtongning Capsule by UPLC-Q-Exactive-MS/MS |
| ZHU Lihua,HUANG Shengwu,SHEN Bingbing,XIE Yi |
| (Hunan Guohua Pharmaceutical Co., Ltd., Changsha, Hunan 410013, China;Hunan Academy of Chinese Medicine, Changsha, Hunan 410013, China) |
| Abstract: |
| Objective To develop a method of UPLC-Q-Exactive-MS/MS for the determination of aristolochic acid Ⅰ in Shangtongning Capsule. Methods The chromatography was performed on Hypersil GOLD C18 column (2.1 mm×50 mm, 1.9 μm) with mobile phases consisting of acetonitrile and 0.1% formic acid aqueous solution (containing 5 mmol/L ammonium formate) at a gradient elution rate of 0.5 mL/min, and the column temperature was 30℃. Electrospray ionization in positive ionization mode was used for parallel reaction monitoring, and ion pairs with mass-to-charge ratios (m/z) of 359.0→298.0 and 359.0→296.0 were selected for monitoring. Results Aristolochic acid Ⅰ had a good linear relationship in the range of 0.06-0.2 ng (R2=0.999 5), RSDs of precision and stability were less than 3%, and the average recovery was 104.1% (RSD=4.29%). The average content of aristolochic acid Ⅰ in different batches of Shangtongning Capsule was 0.000 004 90%, the mean transfer rate from medicinal materials to finished products was 103.7% and RSD was 19.5%. Conclusion With high specificity, sensitivity, and accuracy, the method is reliable and reproducible, and can be used for the determination of aristolochic acid Ⅰ in Shangtongning Capsule. |
| Key words: Shangtongning Capsule aristolochic acid Ⅰ UPLC-Q-Exactive-MS/MS quantitative analysis |
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