超高效液相色谱-三重四极杆质谱法同时测定消肿膏中6种乌头型生物碱含量  

Simultaneous determination of 6 aconitum-type alkaloids in Xiaozhong ointment by ultra-high performance liquid chromatography triple quadrupole mass spectrometry

作　　者：夏天利 赵德萍 薛傲 金美玲 朱紫悦 李卿[3] 张宁[2] 雷霞 XIA Tian-li;ZHAO De-ping;XUE Ao;JIN Mei-ling;ZHU Zi-yue;LI Qing;ZHANG Ning;LEI Xia(College of Pharmacy,Jiamusi University,Jiamusi 154007,Heilongjiang Province,China;The Chinese Medicine Institute,Heilongjiang University of Traditional Chinese Medicine,Harbin 150040,Heilongjiang Province,China;Jiangsu MC Clinical Innovation Center of Degenerative Bone&Joint Disease,Wuxi Hospital of TraditionalChinese Medicine,Wuxi 214071,Jiangsu Province,China)

机构地区：[1]佳木斯大学药学院,黑龙江佳木斯154007 [2]黑龙江中医药大学中医药研究所,黑龙江哈尔滨150040 [3]无锡市中医医院江苏省中医退行性骨关节病临床医学创新中心,江苏无锡214071

出　　处：《中国临床药理学杂志》2024年第9期1341-1344,共4页The Chinese Journal of Clinical Pharmacology

基　　金：江苏省中医退行性骨关节病临床医学创新中心基金资助项目(苏中医科教[2021]4号)。

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,1.7μm),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5μL;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、0.06μg·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。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,1.7μm),mobile phase 0.1%formic acid water(A)-acetonitrile(B),gradient elution,column temperature 40℃,flow rate 0.3 mL·min^(-1),injection volume 5μL;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.

关 键 词：消肿膏 乌头型生物碱 超高效液相色谱-三重四极杆质谱法 含量测定 

分 类 号：R28[医药卫生—中药学]