首页|HPLC法同时测定风湿骨痛片中12个乌头碱类成分的含量

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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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 5μg、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.
Determination of 12 aconite alkaloids in Fengshi Gutong tablets by HPLC
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 245 nm 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 Feng-shi Gutong tablets to achieve comprehensive quality control of preparations.

Fengshi Gutong tabletsaconitinebulleyaconitine AHPLCquality control

卢虹妃、倪倩、冯有龙

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中国药科大学,南京 211198

江苏省食品药品监督检验研究院,南京 210019

风湿骨痛片 乌头碱 草乌甲素 高效液相色谱 质量控制

江苏省市场监督管理局科研计划项目

KJ204121

2024

药物分析杂志
中国药学会

药物分析杂志

CSTPCD北大核心
影响因子:1.039
ISSN:0254-1793
年,卷(期):2024.(9)
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