摘要
目的采用气相色谱-质谱联用技术(GC-MS/MS)测定加味西黄丸中麝香酮的含量,为加味西黄丸的质量控制提供依据。方法色谱条件:色谱分离采用HP-5MS毛细管色谱柱(30 m×0.25 mm,0.25μm),程序升温(初始温度150℃,保持0.5 min,以25℃/min速率升温至200℃,保持5.5 min,以15℃/min速率升温至250℃,保持1 min),载气为高纯氦气,流速为1 mL/min,进样量为1μL,分流比为10∶1;质谱条件:采用电子轰击源(EI源),轰击电压为70 eV,进样口温度为250℃,离子源温度为230℃,四极杆温度为150℃,辅助接口温度为290℃;采用多重反应监测模式对麝香酮和内标(异补骨脂素)进行测定,用于麝香酮和内标检测的离子对及碰撞能量分别为:m/z 238.1→m/z 98.0(CE=10 eV)、m/z 186.2→m/z 158.0(CE=15 eV),溶剂延迟时间为3 min。结果麝香酮保留时间为7.6 min,内标保留时间为6.6 min,麝香酮浓度在0.25~8 mg/L范围内与峰面积比值(麝香酮/内标)呈良好的线性关系,标准曲线回归方程为Y=2.63×10^(-1)X-5.57×10^(-3)(r=0.9991,n=6),精密度、稳定性、重复性的RSD值均在3.0%以内,平均回收率为98.5%,6批样品中麝香酮的含量范围为1.37~1.53 mg/g。结论本研究建立的GC-MS/MS方法简便可行,专属性强、灵敏度高,可为加味西黄丸的质量控制提供参考。
Objective To determine the content of muscone in Modified Xihuang Pills by gas chromatography-mass spectrometry(GCMS/MS),and to provide the basis for the quality control.Methods Chromatographic conditions:The chromatographic separation was per⁃formed on a HP-5MS capillary column(30 m×0.25 mm,0.25μm)with a programmed heating method(initial temperature of 150℃,maintained for 0.5 min,heated at a rate of 25℃/min to 200℃,maintained for 5.5 min,heated at a rate of 15℃/min to 250℃,main⁃tained for 1 min).The carrier gas was high purity helium and the flow rate was 1 mL/min.The injection volume was 1μL and the split ra⁃tio was 10:1.Mass spectrometry conditions:Electron Impact Ionization source(EI source)was used.The bombardment voltage was 70.0 eV,and the inlet temperature was maintained at 250℃.The ion source temperature was 230℃,the quadrupole temperature was 150℃,and the auxiliary interface temperature was 290℃.Multiple reaction monitoring mode was used to determine muscone and internal stan⁃dard(isopsoralen).The ion pair and collision voltage used for detection of muscone and internal standard were as follows:m/z 238.1→m/z 98.0(CE=10 eV),m/z 186.2→m/z 158.0(CE=15 eV),and solvent delay time was 3 min.Results The retention time of mus⁃cone and internal standard was 7.6 min and 6.6 min,respectively.The concentration of muscone showed a good linear relationship with the peak area ratio(muscone/internal standard)within the range of 0.25-8 mg/L.The regression equation of standard curve was Y=2.63×10^(-1)X-5.57×10^(-3)(r=0.9991,n=6).The RSD values of precision,stability and repeatability were all less than 3.0%,and the average re⁃covery was 98.5%,and the content range of muscone in 6 batches of samples was 1.37-1.53 mg/g.Conclusion The established GC-MS/MS method is simple and feasible,with strong specificity and high sensitivity,which can provide reference for the quality control of Modi⁃fied Xihuang Pills.
作者
杨艳
王星
李玉华
于文杰
刘杨
李乐乐
关皎
于春宇
朱鹤云
YANG Yan;WANG Xing;LI Yuhua;YU Wenjie;LIU Yang;LI Lele;GUAN Jiao;YU Chunyu;ZHU Heyun(School of Pharmacy,Yanbian University,Yanji,Jilin Province 133002;School of Pharmacy,Jilin Medical University,Jilin City,Jilin Province 132013;Jilin Jibang Pharmaceutical Co.,Ltd.,Shulan,Jilin Province 132600,China)
出处
《吉林医药学院学报》
2025年第4期249-252,257,共5页
Journal of Jilin Medical University
基金
吉林省科技厅项目(YDZJ202301ZYTS188)。
关键词
加味西黄丸
麝香酮
气相色谱-质谱联用技术
含量测定
Modified Xihuang Pills
muscone
gas chromatography-mass spectrometry
content determination
