标准研讨

HPLC法同时测定风湿骨痛片中12个乌头碱类成分的含量*

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  • 1.中国药科大学,南京 211198;
    2.江苏省食品药品监督检验研究院,南京 210019
第一作者 Tel:15305186790;E-mail:3321020783@stu.cpu.edu.cn
**Tel:13851496828;E-mail:13851496828@163.com

修回日期: 2024-06-11

  网络出版日期: 2024-10-17

基金资助

*江苏省市场监督管理局科研计划项目(KJ204121)

Determination of 12 aconite alkaloids in Fengshi Gutong tablets by HPLC*

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  • 1. China Pharmaceutical University, Nanjing 211198, China;
    2. Jiangsu Institute for Food and Drug Control,Nanjing 210019, China

Revised date: 2024-06-11

  Online published: 2024-10-17

摘要

目的: 建立风湿骨痛片中乌头碱类成分的含量测定方法。方法: 采用Waters XSelectCSH C18色谱柱(250 mm×4.6 mm,5 μm),以0.1%醋酸水溶液-乙腈-甲醇系统为流动相进行梯度洗脱,流速1.0 mL·min-1,检测波长245 nm,柱温30 ℃。结果: 冉乌头碱、苯甲酰新乌头原碱、苯甲酰乌头原碱、苯甲酰次乌头原碱、8-去乙酰基滇乌碱、10-羟基新乌头碱、新乌头碱、次乌头碱、印乌头碱、乌头碱、滇乌头碱、草乌甲素的进样量分别在0.022 8~0.136 6 μg、0.041 5~0.249 0 μg、0.033 5~0.200 8 μg、0.033 9~0.203 1 μg、0.033 1~0.198 6 μg、0.040 3~0.241 6 μg、0.030 2~0.181 4 μg、0.028 6~0.171 6 μg、0.033 6~0.201 6 μg、0.030 3~0.181 9 μg、0.063 4~0.381 5 μg、0.034 0~0.204 2 μg时,其峰面积与进样量呈现良好的线性关系;精密度、重复性、稳定性试验结果均满足有关技术要求;上述12个乌头碱类成分的平均回收率分别在93.6%~101.5%,RSD分别在0.55%~3.3%。3批风湿骨痛片(批号211227、220823、230425)中冉乌头碱、苯甲酰新乌头原碱、苯甲酰乌头原碱、苯甲酰次乌头原碱、8-去乙酰基滇乌碱、10-羟基新乌头碱、新乌头碱、次乌头碱、印乌头碱、滇乌头碱的每片平均含量为0.492、65.78、7.319、10.164、1.068、5.583、2.573、5.865、2.021、2.050 μg;乌头碱、草乌甲素未检出。结论: 所建立的方法专属性强、灵敏度和准确度均较高,可用于风湿骨痛片中12个乌头碱类成分的含量测定,实现对制剂进行全面的质量控制。

本文引用格式

卢虹妃, 倪倩, 冯有龙 . HPLC法同时测定风湿骨痛片中12个乌头碱类成分的含量*[J]. 药物分析杂志, 2024 , 44(9) : 1578 -1585 . DOI: 10.16155/j.0254-1793.2023-0584

Abstract

Objective: To establish a method for determination of aconite alkaloids in Fengshi Gutong tablets. Methods: Analysis was performed on a WatersXSelect CSH C18(250 nm×4.6 mm, 5 μm) column with mobile phase consisting of 0.1% acetic acid aqueous solution, acetonitrile and methanol with gradient elution at a flow rate of 1.0 mL·min-1. The detection wavelength was set at 245nm and the column temperature was 30 ℃. Results: Twelve aconite alkaloids could be separated well. When the injection amounts of ranaconitine, benzoylmesaconine, benzoylmesaconine, benzoylmesaconine, acoforestinine and beiwutine, mesaconitine, hypaconitine, indaconitine, aconitine, yunaconitine, bulleyaconitine A were 0.022 8-0.136 6 μg, 0.041 5-0.249 0 μg, 0.033 5-0.200 8 μg, 0.033 9-0.203 1 μg, 0.033 1-0.198 6 μg, 0.040 3-0.241 6 μg, 0.030 2-0.181 4 μg, 0.028 6-0.171 6 μg, 0.033 6-0.201 6 μg, 0.030 3-0.181 9 μg, 0.063 4-0.381 5 μg and 0.034 0-0.204 2 μg, respectively, the peak area showed a good linear relationship with the injection amounts. The average recovery rates of 12 aconite alkaloid components ranged from 93.6% to 101.5%, and the RSD ranged from 0.55% to 2.6%. The average contents of ranaconitine, benzoylmesaconine, benzoylmesaconine, benzoylmesaconine, acoforestinine and beiwutine, mesaconitine, hypaconitine, indaconitine and yunaconitine in three batches of Fengshi Gutong tablets (batch No. 211227, 220823 and 230425) were 0.492 μg, 65.78 μg, 7.319 μg, 10.164 μg, 1.068 μg, 5.583 μg, 2.573 μg, 5.865 μg, 2.021 μg, 2.050 μg, respectively. And aconitine and bulleyaconitine A were not detected. Conclusions: The established method is accurate and reliable, and can be used for the determination of 12 aconite alkaloids compounds in Fengshi Gutong tablets to achieve comprehensive quality control of preparations.

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