摘要
目的 用超高效液相色谱-三重四极杆质谱串联(UPLC-TQD-MS)法同时测定消肿膏中乌头碱、新乌头碱、次乌头碱、苯甲酰乌头原碱、苯甲酰新乌头原碱、苯甲酰次乌头原碱的含量.方法 用ACQUITY UPLC BEH C18柱(50 mm × 2.1 mm,1.7 µm),流动相为0.1％甲酸水(A)-乙腈(B),梯度洗脱,柱温为40℃,流速为0.3 mL·min-1,进样量5 µL;用电喷雾离子源正离子模式(ESI+)和多反应监测模式(MRM)进行质谱分析.结果 乌头碱、新乌头碱、次乌头碱、苯甲酰乌头原碱、苯甲酰新乌头原碱、苯甲酰次乌头原碱的质量浓度均在1.0～100.0 ng·mL-1呈良好线性关系,平均加样回收率为98.62％～101.24％.3个批样品中,6个成分的质量分数分别为0.18、0.33、0.38、0.43、0.28、0.06 μg·g-1.结论 该方法可用于检测消肿膏中6种乌头型生物碱含量,为消肿膏的质量评价及临床安全用药提供参考.
Abstract
Objective To establish a method for the simultaneous determination of aconitine,neoaconitine,hypaconitine,benzoyl aconitine,benzoyl mesaconine and benzoylhypacoitine in Xiaozhong ointment by UPLC-TQD-MS.Methods ACQUITY UPLC BEH C18 column(50 mm ×2.1 mm,1.7 μm),mobile phase 0.1％formic acid water(A)-acetonitrile(B),gradient elution,column temperature 40 ℃,flow rate 0.3 mL·min-1,injection volume 5 μL;electrospray ionization source(ESI+)and multiple reaction monitoring(MRM)were used for mass spectrometry analysis.Results The concentration of aconitine,new aconitine,hypaconitine,benzoyl aconitine,benzoyl new aconitine and benzoyl hypaconitine were 1.0-100.0 ng·mL-1,respectively,the average recovery were 98.62％-101.24％.The mass fractions of the six components were 0.18,0.33,0.38,0.43,0.28,0.06μg·g-1.Conclusion The method can be used to determine the content of 6 aconitine-type alkaloids in Xiaozhong ointment,and provide reference for the quality evaluation and clinical safe use of Xiaozhong ointment.
基金项目
江苏省中医退行性骨关节病临床医学创新中心项目(苏中医科教[2021]4号)
国家科技期刊平台
NSTL
万方数据