摘要
[目的]采用超高液相色谱-串联质谱(UPLC-MS/MS)技术建立可同时测定醒脑静注射液中莪术二酮、吉马酮、左旋樟脑、姜黄素和麝香酮5种指标性成分含量的新方法。[方法]研究项下使用的色谱柱为ACQUITY HSS^(■)T3C_(18)柱(2.1 mm×100 mm,1.8μm),流动相A为0.1%甲酸水溶液+2 mmol乙酸铵,流动相B为甲醇溶液+0.1%甲酸。梯度洗脱方法:0~0.5 min,95%A;0.5~1.0 min,95%→5%A;1.0~2.7 min,5%A;2.7~3.4 min,5%→95%A;3.4~4.0 min,95%A。流速:0.4 mL/min;柱温:40℃;进样量:5μL;采用电喷雾离子源进行正离子监测,多反应监测模式(MRM)用于定量分析。[结果]在4 min内,醒脑静注射液的5个标志性成分,包括莪术二酮、吉马酮、左旋樟脑、姜黄素和麝香酮被完全分离,峰面积与浓度呈现出良好的线性关系,相关系数(r)均大于0.9980。对该检测方法的精密度、重复性和稳定性进行评价,均得到了满意结果。平均加样回收率为98.2%~104.2%。6批样品中莪术二酮、吉马酮、左旋樟脑、姜黄素和麝香酮含量测定结果分别为19.4~20.4、1.6~1.8、29.0~31.0、1.3~1.4、11.6~12.4μg/mL。[结论]该检测方法具有高灵敏度、准确可靠的优势,可实现对醒脑静注射液中多个组分快速检测,为该制剂的质量控制研究提供了参考。
[Objective]A new method for simultaneous determination of 5 index components containing curcuma dione,gemarone,L-camphor,curcumin and muscosterone in Xingnaojing Injection was established by ultra high liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).[Methods]The chromatographic column used in this research was ACQUITY HSS^(■)T3 C_(18) column(2.1 mm×100 mm,1.8μm).The mobile phase consisted of 0.1%formic acid water and 2 mmol ammonium acetate(A),methanol and 0.1%formic acid(B)with gradient elution(0 to 0.5 min,95%A;0.5 to 1.0 min,95%to 5%A;1.0 to 2.7 min,5%A;2.7 to 3.4 min,5%→95%A;3.4 to 4.0 min,95%A).The injection volume was 5μL and the flow rate was 0.4 mL/min.The column temperature was 40℃.Electrospray ion source was adopted for positive ion monitoring,and multi-reaction monitoring mode(MRM)was used for quantitative analysis.[Results]Within 4 min,the five signature components of Xingnaojing Injection,including curcuma dione,jimarone,L-camphor,curcumin and muscatone,were completely separated.The peak area showed a good linear relationship with the concentration,and the correlation coefficient(r)was greater than 0.9980.The accuracy,repeatability and stability of the method were evaluated,and satisfactory results were obtained.The average recoveries were 98.2%to 104.2%.The contents of curcuma dione,jimarone,L-camphor,curcumin and muscatone in 6 batches of samples were 19.4 to 20.4,1.6 to 1.8,29.0 to 31.0,1.3 to 1.4,11.6 to 12.4μg/mL,respectively.[Conclusion]The method has the advantages of high sensitivity,accuracy and reliability,and can realize the rapid detection of multiple components in Xingnaojing Injection,which provides a reference for the quality control research of this preparation.
作者
王沫初
付娜静
石艳丽
陈卓
王传琦
李爽
孟凡爽
姚蒙蒙
姜晖
WANG Mochu;FU Najing;SHI Yanli;CHEN Zhuo;WANG Chuanqi;LI Shuang;MENG Fanshuang;YAO Mengmeng;JIANG Hui(Tangshan Central Hospital,Tangshan 063000,China;Jitang College of North China University of Science and Technology,Tangshan 063000,China)
出处
《天津中医药》
CAS
2024年第9期1187-1191,共5页
Tianjin Journal of Traditional Chinese Medicine
基金
河北省中医药管理局2022年度中医药类科研计划项目(2022562)。
